I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[38206]
Open Access
Abstract: Masonry structures predominantly work under compression; elasticity in constituent materials is therefore typically characterised during uniaxial compression tests via load and deformation measurements. In most practical applications, deformation measurements can only be conducted at the surface of the sample. To understand the influence of this restriction on characterisation results, this study conducts in-situ load tests on hydraulic lime mortar samples with both surface and volumetric imaging, using stereo cameras and synchrotron X-rays. The imaging data are processed with Digital Image and Volume Correlation algorithms (local and global) to obtain full-field displacements and strains. Deformation measurements are then used to conduct surface characterisation with the Virtual Fields Method (VFM) and volumetric characterisation with Finite Element Model Updating (FEMU). Since the inverse models indicate limited identifiability for Poisson’s ratio, only the Young’s moduli are compared. Results indicate that accurate Young’s moduli can be obtained from surface measurements, provided that through-thickness load gradients are considered by averaging VFM results from front and back faces of the sample. In addition, it is shown that a surface characterisation domain away from contacts needs to be chosen to ensure that surface strains are representative of bulk behaviour. Finally, a systematic reduction of elastic moduli with increasing loads is observed, suggesting damage development at relatively low stress levels in hydraulic lime mortars.
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Sep 2026
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[11204]
Open Access
Abstract: Background/Objectives: Trabecular bone exhibits brittle behaviour governed by microscale deformation and damage, yet quantifying crack progression is difficult because classical fracture-mechanics approaches do not apply to architecturally discontinuous porous tissue. This pilot study evaluates whether synchrotron X-ray computed tomography (XCT) combined with digital volume correlation (DVC) can provide a practical, geometry-normalised approach for quantifying crack-opening behaviour in human trabecular bone. Methods: Semicylindrical specimens from femoral heads of hip-fracture donors (n = 5) and non-fracture controls (n = 5) underwent stepwise three-point bending during XCT imaging. Full-field displacement maps were used to measure crack mouth opening displacement (CMOD), crack length (a), and their ratio CMOD/a, used here as a geometry-normalised comparative descriptor of brittle response rather than an intrinsic material property. Automated phase-congruency crack detection (PCCD) was compared with manual measurement. Results: XCT–DVC resolved three-dimensional displacement discontinuities during crack initiation and propagation in all specimens. Hip-fracture donors exhibited significantly lower critical crack-opening ratios (CMOD/a)* than Controls (median 0.31 vs. 0.47; p = 0.008) and reached instability at lower applied loads. Total crack extension (Δa*) was similar between groups. Automated crack tracking using phase-congruency-based segmentation showed excellent agreement with manual measurements (r2 = 0.98), supporting reliable extraction of crack geometry from DVC displacement fields. Conclusions: In this small pilot sample, XCT–DVC provided a feasible, geometry-normalised approach for comparing crack-opening behaviour where classical fracture-mechanics parameters cannot be applied. The close agreement between automated and manual crack measurements supports the reproducibility of the displacement-based measurement pipeline. The lower critical CMOD/a in hip-fracture specimens may indicate a more brittle comparative response. However, given the small sample, differing sex distribution, and lower bone volume fraction in the hip-fracture group, these findings are preliminary and require confirmation in larger cohorts. Establishing whether the observed difference reflects intrinsic tissue brittleness, architectural factors, or both is an important objective for future work in microstructure-matched cohorts.
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Jul 2026
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[34540]
Open Access
Abstract: Fibrous plaster (FP) is a fabric-reinforced composite (FRC) comprising plaster of Paris (POP) and woven jute fabric (‘hessian’), historically used in decorative ceilings across the UK since the late 19th century. Despite its architectural significance, FP remains under-researched, limiting the development of reliable structural assessment methods. Recent ceiling failures have been linked to the tensile failure of the supporting component known as the ‘wad’. Acoustic emission (AE) provides a non-destructive means of remotely sensing and locating such failures from the underside of ceilings, yet its potential for extracting detailed information on FP wad failure processes remains unexplored. This study comprises two parts. First, an AE-based failure classification model was developed using unsupervised spherical k-means clustering to distinguish matrix cracking and fabric–matrix debonding based on the RA-AF method. Second, the first in-situ direct tensile tests on FP wad-analogue specimens conducted under synchrotron X-ray imaging were conducted at the I12 beamline of Diamond Light Source (DLS), UK, integrating AE monitoring with digital image correlation (DIC) and synchrotron X-ray computed tomography (sCT). This multi-modal dataset enabled examination of the AE model and internal failure analysis through digital volume correlation (DVC), while complementary crack analysis and the Kabsch algorithm provided new insight into the failure mechanisms of FP wads and revealed the reinforcement-bridging role of the hessian during progressive fracture. By linking remote AE monitoring with multi-scale observations, this study advances understanding of FP failure processes, offering a pathway for assessing historic ceilings and informing the design of more resilient FP components.
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Jun 2026
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DIAD-Dual Imaging and Diffraction Beamline
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Diamond Proposal Number(s):
[33351]
Abstract: Utilizing green and renewable materials derived from biological sources is crucial for reducing environmental pollution. Natural wood is a clean and sustainable material. Densification methods have been shown to greatly enhance the mechanical properties of wood. However, the inherent hydrophilic and hygroexpansion characteristics of wood significantly limit the application of densified wood in various engineering fields. This study aimed to investigate the water absorption behavior and dimensional stability of natural and densified pine through water absorption experiments. The results showed that densified pine exhibited a similar three-stage water absorption behavior to that of natural pine. The water absorption behavior of densified pine caused by diffusion of water molecules as bound water in the cell wall (stage I), conforming to the Fickian model. In the subsequent stage II, excess water in the cell wall diffused into the cell lumen as free water. The water absorption behavior then deviated from the Fickian model and followed the Langmuir model. The significant reduction in the equilibrium moisture content of densified pine, compared to natural pine, can be attributed to a decrease in hemicellulose as well as smaller cell interstices and lumens. Moreover, unlike natural pine, where hygroexpansion was only in stage Ⅰ, densified pine expanded further in stage Ⅱ due to partial recovery of the cell lumen. Nuclear magnetic resonance (NMR), Fourier-transform infrared (FT-IR), Scanning electron microscopy (SEM) and X-ray computed tomography and diffraction techniques were employed to elucidate the effect of densification on dimensional stability and water absorption behavior of pine.
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Apr 2026
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DIAD-Dual Imaging and Diffraction Beamline
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Abstract: Anode-free solid-state batteries (AF-SSBs) hold great promise for next-generation transportation electrification, offering improved safety, recyclability, and high performance (energy density >1500 Wh/L, specific energy >500 Wh/kg) at reduced cost (<$100/kWh) compared to conventional Li-ion batteries. However, their practical deployment is hindered by poor chemo-mechanical stability at the evolving anode|solid electrolyte (SE) interface, where localized ionic flux during cycling drives dendrite formation, internal short-circuiting, and premature failure. The buried and dynamic nature of this interface makes direct characterization especially challenging, and existing methods lack the ability to capture non-invasive, 3D operando insights into interfacial morphology, spatial dynamics, and strain evolution in full-cell AF-SSBs.
In this work, we conducted operando correlative synchrotron X-ray micro-computed tomography (XCT) and X-ray diffraction (XRD) at the DIAD beamline, Diamond Light Source (UK), to map interface evolution in real time. Custom PEEK-housed tube cells were cycled at 35 µA (2 mm Li | 19 mg LPSC | 3 mm stainless steel), with 13 tomographic scans collected across three charge–discharge cycles prior to short-circuiting. XCT resolved void formation, crack initiation, and fracture propagation, while XRD provided spatially resolved strain mapping and crystallographic fingerprints of interfacial contact evolution.
Our imaging data revealed pre-existing cracks within the SE pellet, as well as the nucleation of new spallation-like cracks originating at the current collector–SE interface that widened progressively during cycling. XRD mapping confirmed that these cracks coincided with regions of strain accumulation and interfacial delamination, offering a crystallographic fingerprint of contact evolution. Importantly, these structural changes could be directly correlated with electrochemical signatures: the onset of fracture formation aligned with abrupt cell polarization and preceded catastrophic short-circuiting. Together, this correlative XCT–XRD methodology provides the integrated view of how morphology, strain, and electrochemistry couple to govern failure in AF-SSBs.
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Mar 2026
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DIAD-Dual Imaging and Diffraction Beamline
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Loris
Chavée
,
Emile
Haye
,
Jochen M.
Schneider
,
Stanislav
Mráz
,
Andreas
Pflug
,
Dennis
Barton
,
Armel
Descamps
,
Claudie
Josse
,
Jérôme
Müller
,
Pavel
Moskovkin
,
James
Marrow
,
Amael
Caillard
,
Stephane
Lucas
Diamond Proposal Number(s):
[34010]
Abstract: The deposition of functional coatings on open-cell foam substrates using magnetron
sputtering is gaining popularity, particularly for applications like Oxygen Evolution
Reaction (OER)/Hydrogen Evolution Reaction (HER) catalysis, batteries, and
supercapacitors. While most research focuses on performance, little attention has
been paid to the coating growth mechanisms or properties within the foam, which could
significantly impact device performance. This work investigates the properties and
growth mechanisms of TiO₂ coatings inside porous foams, using experimental and
modeling techniques.
The structure, composition and thickness of the coating on the outermost surface of
the foam are studied using Focused Ion Beam (FIB), Scanning Transmission Electron
Microscopy (STEM), Energy-Dispersive X-Ray Spectroscopy (EDS), Selected Area
Electron Diffraction (SAED) and High-Resolution Transmission Electron Microscopy
(HRTEM). The experimental results reveal the formation of a dense, (quasi-
)stoichiometric and crystalline coating.
Numerical simulations and experiments highlight the transport of plasma particles in
the foam. Interestingly, Direct Simulation Monte Carlo (DSMC)/Particle-In-Cell Monte
Carlo (PICMC) models, coupled with Mass-Energy Analyzer (MEA) experiments,
demonstrate that the particle flux is reduced, but the particle energy distribution is not
Accepted Manuscript affected while traveling inside the foam. Using kinetic Monte Carlo (kMC) thin film
growth models provided by Virtual CoaterTM, the physical properties of the coating
inside the foam have been modeled, and the drop in coating thickness as well as the
impact of bias voltage on densification, resistivity, and optical absorption are
confirmed. Synchrotron X-Ray Diffraction (SXRD) analyses of the foam demonstrate
that the same crystalline phase is obtained along the foam thickness, but it can be
tailored with bias voltages. The decrease in the recorded SXRD signal with increasing
depth inside the foam also suggests a drop in coating thickness.
The new insights on the properties of coatings inside open-cell foams presented in this
study can be used to improve future foam-based devices.
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Dec 2025
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I13-2-Diamond Manchester Imaging
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Dominic L. R.
Melvin
,
Marco
Siniscalchi
,
Dominic
Spencer-Jolly
,
Bingkun
Hu
,
Ziyang
Ning
,
Shengming
Zhang
,
Junfu
Bu
,
Shashidhara
Marathe
,
Anne
Bonnin
,
Johannes
Ihli
,
Gregory J.
Rees
,
Patrick S.
Grant
,
Charles W.
Monroe
,
T. James
Marrow
,
Guanchen
Li
,
Peter G.
Bruce
Diamond Proposal Number(s):
[30683]
Open Access
Abstract: Avoiding lithium dendrites at the lithium/ceramic electrolyte interface and, as a result, avoiding cell short circuit when plating at practical current densities remains a significant challenge for all-solid-state batteries. Typically, values are limited to around 1 mA cm−2, even, for example, for garnets with a relative density of >99%. It is not obvious that simply densifying ceramic electrolytes will deliver high plating currents. Here we show that plating currents of 9 mA cm−2 can be achieved without dendrite formation, by densifying argyrodite, Li6PS5Cl, to 99%. Changes in the microstructure of Li6PS5Cl on densification from 83 to 99% were determined by focused ion beam-scanning electron microscopy tomography and used to calculate their effect on the critical current density (CCD). Modelling shows that not all changes in microstructure with densification act to increase CCD. Whereas smaller pores and shorter cracks increase CCD, lower pore population and narrower cracks act to decrease CCD. Calculations show that the former changes dominate over the latter, predicating an overall increase in CCD, as observed experimentally.
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Sep 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Jiaxu
Zuo
,
Kutsi
Akcicek
,
Shivansh
Nauriyal
,
Barrie
Dams
,
Stefan
Michalik
,
Thomas
Zillhardt
,
Martin
Ansell
,
Richard
Ball
,
Genoveva
Burca
,
Brian
Sheil
,
James
Marrow
,
Sinan
Acikgoz
Open Access
Abstract: Fibrous plaster (FP) ceilings, prevalent in late 19th- and early 20th-century UK theatres, are suspended using ‘wads’. Wads are hangers made of Plaster of Paris, reinforced with twisted woven jute fabric. Several recent collapses in historic fibrous plaster ceilings have been attributed to tensile failures in wads. To understand the failure mechanisms involved, tensile tests were performed on laboratory-produced wad-like samples at the I12 beamline of the UK Diamond Light Source. The tested samples were designed with a dog bone shape and mounted with clevis-grips at each end, to ensure controlled failures along the gauge length. The beamline offered the opportunity to conduct simultaneous synchrotron X-ray computed tomography (sCT) and diffraction measurements during loading, enabling the monitoring of internal crack formation and strain propagation at the microstructural scale. Simultaneously, acoustic emission (AE) and digital image correlation (DIC) measurements were conducted. Preliminary results from these datasets are discussed in this paper. The datasets will provide useful information to validate the ongoing development of algorithms which can categorise the internal failure mechanisms and damage state of wads using only AE signals.
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Sep 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
I13-2-Diamond Manchester Imaging
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Bingkun
Hu
,
Shengming
Zhang
,
Ziyang
Ning
,
Dominic
Spencer-Jolly
,
Dominic L. R.
Melvin
,
Xiangwen
Gao
,
Johann
Perera
,
Shengda D.
Pu
,
Gregory J.
Rees
,
Longlong
Wang
,
Lechen
Yang
,
Hui
Gao
,
Shashidhara
Marathe
,
Genoveva
Burca
,
T. James
Marrow
,
Peter G.
Bruce
Diamond Proposal Number(s):
[26060, 30683, 28773]
Open Access
Abstract: Charging current densities of solid-state batteries with lithium metal anodes and ceramic electrolytes are severely limited due to lithium dendrites that penetrate the electrolyte leading to a short circuit. We show that dendrite growth can be inhibited by different crack deflection mechanisms when multi-layered solid electrolytes, such as Li6PS5Cl/Li3ScCl6/Li6PS5Cl and Li6PS5Cl/Li10GeP2S12/Li6PS5Cl, are employed but not when the inner layer is Li3PS4. X-ray tomographic imaging shows crack deflection along mechanically weak interfaces between solid electrolytes as a result of local mismatches in elastic moduli. Cracks are also deflected laterally within Li3ScCl6, which contains preferentially oriented particles. Deflection occurs without lithium being present. In cases where the inner layers react with lithium, the resulting decomposition products can fill and block crack propagation. All three mechanisms are effective at low stack pressures. Operating at 2.5 MPa, multi-layered solid electrolytes Li6PS5Cl/Li3ScCl6/Li6PS5Cl and Li6PS5Cl/Li10GeP2S12/Li6PS5Cl can achieve lithium plating at current densities exceeding 15 mA cm−2.
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Jul 2024
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Open Access
Abstract: The capacity of polygranular graphite to accommodate strain is important to its use within structural components. This study has used in situ neutron and synchrotron X-ray experiments to demonstrate that reorientation of crystal domains accompanies the accommodation of applied mechanical strain in unirradiated Gilsocarbon (GCMB/IM24) graphite. Orientation changes were observed using 3D X-ray Diffraction, and local changes in neutron scattering were also observed with energy-resolved Bragg-edge neutron imaging. In both cases, this behaviour at the crystal level was partially recovered when the load was removed. This study provides new evidence for crystal deformation mechanisms that contribute to polycrystalline graphite's elastic non-linearity and the development of permanent set, which may also explain the effects of fast neutron irradiation on graphite elastic behaviour.
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Aug 2023
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