I13-2-Diamond Manchester Imaging
|
Xuekun
Lu
,
Rhodri
Owen
,
Wenjia
Du
,
Zhenyu
Zhang
,
Antonio
Bertei
,
Roby
Soni
,
Xun
Zhang
,
Francesco
Iacoviello
,
Daqing
Li
,
Alice
Llewellyn
,
Jianuo
Chen
,
Han
Zhang
,
Xuhui
Yao
,
Qi
Li
,
Yunlong
Zhao
,
Shashidhara
Marathe
,
Christoph
Rau
,
Paul R.
Shearing
Diamond Proposal Number(s):
[29068]
Open Access
Abstract: Silicon is a promising negative electrode material for high-energy batteries, but its volume changes during cell cycling cause rapid degradation, limiting its loading to about 10 wt.% in conventional graphite/Si composite electrodes. Overcoming this threshold requires evidence-based design for the formulation of advanced electrodes. Here we combine multimodal operando imaging techniques, assisted by structural and electrochemical characterizations, to elucidate the multiscale electro-chemo-mechanical processes in graphite/Si composite negative electrodes. We demonstrate that the electrochemical cycling stability of Si particles strongly depends on the design of intraparticle nanoscale porous structures, and the encapsulation and loss of active Si particles result in excessive charging current being directed to the graphite particles, increasing the risk of lithium plating. We also show that heterogeneous strains are present between graphite and Si particles, in the carbon-binder domain and the electrode’s porous structures. Focusing on the volume expansion of the electrode during electrochemical cycling, we prove that the rate performance and Si utilization are heavily influenced by the expansion of the carbon-binder domain and the decrease in porosity. Based on this acquired knowledge, we propose a tailored double-layer graphite/Si composite electrode design that exhibits lower polarization and capacity decay compared with conventional graphite/Si electrode formulations.
|
Oct 2025
|
|
I13-2-Diamond Manchester Imaging
|
Diamond Proposal Number(s):
[33620, 38900, 36899]
Abstract: Hearing loss is a prevalent symptom of osteogenesis imperfecta (OI), a group of collagen type I-related skeletal disorders, commonly known as brittle bone disease. Clinical manifestation of hearing loss in OI often presents with stapes footplate fixation and hypodense foci in the otic capsule. However, the etiology and evolution of OI-hearing loss and its relation to bone abnormalities are still unknown. This study investigates the onset, severity, and progression of hearing loss in the homozygous oim mouse model of severe OI Type III, which is reported to exhibit hearing loss at 11-12 weeks of age (Chen et al., 2007), using auditory brainstem responses up to 26 weeks of age. We further examine the presence of deformities, microcracks, and fractures of the ossicular chain using synchrotron microtomography. Our results demonstrate that oim/oim mice have normal hearing, regardless of i) their parental lineage, ii) their husbandry in isolation or with other animals, iii) their mastication with powder or chow food, and iv) their anesthesia with single or multiple ketamine injections. Bone abnormalities like excessive formations, fusions, and fractures, were observed in up to 33% of wild-type and up to 43% of oim/oim mice in each group. Among these, joint and bone-tendon abnormalities were twice as frequent in the oim/oim mice compared to the wild-type mice. Notably, these abnormalities did not impact the hearing response in mice. Whether such bone abnormalities occur and alter auditory function in humans with OI remains uncertain.
|
Jul 2025
|
|
I13-2-Diamond Manchester Imaging
|
Diamond Proposal Number(s):
[22198]
Open Access
Abstract: Solid-state lithium batteries are developing rapidly as a promising next-generation battery, while challenges still persist in understanding their degradation processes during cycling due to the difficulties in characterization. In this study, the 3D morphological evolution of the Li3PS4 solid electrolyte was tracked during electrochemical cycles (plating and stripping) until short circuit by utilizing in situ synchrotron X-ray computed tomography with sufficient spatial and temporal resolution. During the degradation process, cracks in the electrolyte alternately generated from the two electrode/electrolyte interfaces and propagated until shorting. The lithium dendrites filled in the electrolyte cracks but had a greatly reduced filling ratio after the first plating stage; therefore, the cell could continue working for some time after the solid electrolyte was fully fractured by cracks. The compression of the two lithium electrodes mainly occurred in initial cycles where a ca. 4–7 μm reduction in thickness was observed. The mechanical force and electric potential fields were modeled to visualize their redistributions in different stages of cycling. The release of strain energy after the first penetration and thereafter the subsequent driving forces are discussed. These results reveal a fast degradation of solid electrolyte in the initial cycles, providing insights for further modifications and improvements in solid-state batteries.
|
May 2025
|
|
I13-2-Diamond Manchester Imaging
|
Diamond Proposal Number(s):
[20925, 24142]
Abstract: Hearing loss affects approximately 70 % of individuals with osteogenesis imperfecta (OI), a genetic connective tissue disorder characterized by bone fragility and deformities. No effective treatments exist for OI hearing loss, and its etiology is unknown limiting the development of new targeted therapies. This work investigates the impact of OI type I collagen mutations on the ossicle bone properties in the homozygous oim mouse model of severe OI, which is known to exhibit hearing loss. The morphology and porosity of the ossicles of 14-week-old oim and wild-type mice were analyzed using high-resolution synchrotron radiation microtomography. Additionally, the collagen fibers structure, bone tissue composition and mechanical properties were evaluated through second harmonic generation microscopy, Raman spectroscopy, and nanoindentation. The results demonstrated that oim ossicles are small, highly porous with an elevated lacunar number density, a flat stapes footplate and a small malleal processus brevis. One-in-two oim ossicles had incudomalleal joint abnormalities, exhibiting either a localized fracture in the incus head or a joint space widening. No differences were observed in collagen fibers structure, bone tissue composition and mechanical properties. These findings suggest that bone fractures observed in the oim incus may contribute to their reported hearing loss. However, the underlying mechanism for these fracture development remains to be investigated, as they do not appear to result from changes in bone tissue properties (collagen fibers organization, tissue composition or mechanical properties). Instead, they may be associated with joint space widening, and possibly altered ossicle chain kinematics.
|
Apr 2025
|
|
I13-2-Diamond Manchester Imaging
|
Huw C. W.
Parks
,
Matthew
Jones
,
Aaron
Wade
,
Alice
Llewellyn
,
Chun
Tan
,
Hamish
Reid
,
Ralf
Ziesche
,
Thomas M. M.
Heenan
,
Shashidhara
Marathe
,
Christoph
Rau
,
Paul R.
Shearing
,
Rhodri
Jervis
Diamond Proposal Number(s):
[28650]
Open Access
Abstract: To understand fracture behaviour in battery materials, X-ray computed tomography (X-ray CT) has become the primary technique for non-destructive particle and crack analysis. Cracking causes performance decline in polycrystalline NMC811 by exposing new surfaces for parasitic electrolyte reactions and disconnecting active material from the electrode matrix. First cycle crack formation has been documented, but definitive electrochemically induced particle fracture is challenging to assess due to complex sample preparation and high-resolution X-ray imaging requirements. Presented here is an operando X-ray CT technique that enables accurate observation of fracture behaviour during de-/lithiation. A non-linear relationship between fracture behaviour and cell voltage was uncovered, and evidence of particle reformation during re-lithiation. Using a grey level analysis algorithm for fracture detection, we expedite damage evaluation in several thousands of particles throughout the electrochemical process, understanding crack initiation, propagation, and closure on a large, statistical scale and give the ability to track any one of the thousands of particles through its individual electrochemical history. Additionally, we explore the effects of continued volumetric hysteresis on particle damage. For the first time, we demonstrate the complex plurality of fracture behaviour in commercial lithium-ion battery materials, aiding in designing mitigation strategies against particle fracture.
|
Mar 2025
|
|
I13-2-Diamond Manchester Imaging
|
Diamond Proposal Number(s):
[34473]
Open Access
Abstract: Molluscan brains are composed of morphologically consistent and functionally interrogable neurons, offering rich opportunities for understanding how neural circuits drive behavior. Nonetheless, detailed component-level CNS maps are often lacking, total neuron numbers are unknown, and organizational principles remain poorly defined, limiting a full and systematic characterization of circuit operation. Here, we establish an accessible, generalizable approach, harnessing synchrotron X-ray tomography, to rapidly determine the three-dimensional structure of the multimillimeter-scale CNS of Lymnaea. Focusing on the feeding ganglia, we generate a full neuron-level reconstruction, revealing key design principles and revising cell count estimates upward threefold. Our atlas uncovers the superficial but also nonsuperficial ganglionic architecture, reveals the cell organization in normally hidden regions—ganglionic “dark sides”—and details features of single-neuron morphology, together guiding targeted follow-up functional investigation based on intracellular recordings. Using this approach, we identify three pivotal neuron classes: a command-like food-signaling cell type, a feeding central pattern generator interneuron, and a unique behavior-specific motoneuron, together significantly advancing understanding of the function of this classical control circuit. Combining our morphological and electrophysiological data, we also establish a functional CNS atlas in Lymnaea as a shared and scalable resource for the research community. Our approach enables the rapid construction of cell atlases in large-scale nervous systems, with key relevance to functional circuit interrogation in a diverse range of model organisms.
|
Mar 2025
|
|
I13-2-Diamond Manchester Imaging
|
Diamond Proposal Number(s):
[13848, 16052, 17632, 20385]
Open Access
Abstract: Understanding how ecological communities assemble in relation to natural and human-induced environmental changes is critical, particularly for communities of pollinators that deliver essential ecosystem services. Despite widespread attention to interactions between functional traits and community responses to environmental changes, the importance of sensory traits has received little attention. To address this, we asked whether visual traits of bumblebee communities varied at large geographical scales along a habitat gradient of increased tree cover. Because trees generate challenging light conditions for flying insects, in particular a reduced light intensity, we hypothesised that differences in tree cover would correlate with shifts in the visual and taxonomical composition of bumblebee communities. We quantified 11 visual traits across 36 specimens from 20 species of bumblebees using micro-CT and optical modelling of compound eyes and ocelli, and investigated how these traits scale with body size. Using an inventory of bumblebee communities across Sweden and our visual trait dataset, we then explored how visual traits (both absolute and relative to body size) differed in relation to tree cover. We found positive shifts of the community weighted means of visual traits along the increasingly forested habitat gradient (facet diameter, inter-ommatidial angle, eye parameter of the compound eye and alignment of the three ocelli) that were consistent regardless of body size, while other traits decreased when more forest was present in the landscape (facet number). These functional patterns were associated with differences in the abundance of six common species that likely explains the community-wide shift of visual traits along the habitat gradient. Our study demonstrates the interaction between vision, habitat and community assembly in bumblebees, while highlighting a promising research topic at the interface between sensory biology and landscape ecology.
|
Dec 2024
|
|
I13-1-Coherence
I13-2-Diamond Manchester Imaging
|
Christoph
Rau
,
Darren J.
Batey
,
Shashidhara
Marathe
,
Leonard
Turpin
,
Kudakwashe
Jakata
,
Silvia
Cipiccia
,
Isabel
Anthony
,
Roberto
Volpe
,
Claus-Peter
Richter
,
Alessandra
Carriero
,
Maud
Dumoux
,
Jurgen E.
Schneider
,
Erica
Dall'Armellina
,
Marc W.
Holderied
,
Jan
Van Den Bulcke
Open Access
Abstract: We report about the experimental work related to hierarchical structures at the Diamond I13L beamlines. The I13-2 Imaging and I13-1 Coherence beamlines provide imaging with micro- and nano-resolution. The Diamond II upgrade for the synchrotron source and the OCTOPI upgrade for I13L provide new opportunities for expanding the existing scientific areas in multiscale and operando imaging. We describe the scientific research benefitting from the instrumental upgrade. Comparable recording times across all length scales will enable hierarchical operando imaging. With the implementation of automated high-throughput data acquisition and analysis, large numbers of samples will be analyzed.
|
Nov 2024
|
|
I13-2-Diamond Manchester Imaging
|
Diamond Proposal Number(s):
[25254]
Open Access
Abstract: The engineering of biochars with desired morphologies and pore structures is a far-reaching objective towards sustainable pore-dependent environmental technologies, such as water and soil remediation or catalysis. We hereby report a series of experiments that allow the direct following of the shape and porosity of single biochar particles during pyrolysis. Particles ~ 1–2 mm in diameter of unwashed and water-washed raw walnut shells were continuously 3D imaged during pyrolysis to 575 ℃ at a 10 K min−1 in Ar to obtain time- and temperature-resolved x-ray micro computed tomographies to a 0.82 μm resolution. Results showed visual evidence of a 30% and 70% v/v particle shrinkage for unwashed and washed samples, respectively. Particle swelling between 200 and 300 ℃ in the unwashed sample provided evidence of the softening of native biopolymers associated with lignin in untreated biomass. A purpose-defined parameter Λ shows the temperature-dependence of pore re-distribution towards the center of the particle to be linear for both samples. Λ was found to be in the washed sample, approximately 3.5 times faster than in the unwashed one. Such linear dependence is significantly slower than an exponential Arrhenius-like trend thereby providing a qualitative measure of the heat and mass transport phenomena limiting the chemical reactions in the porous medium. This evidence is key to resolving the pathways to the thermochemical decomposition of biomass leading to preparation of precision-engineered biochars.
|
Oct 2024
|
|
I13-1-Coherence
I16-Materials and Magnetism
|
David
Serban
,
Daniel G.
Porter
,
Ahmed H.
Mokhtar
,
Mansoor
Nellikkal
,
Sivaperuma
Uthayakumar
,
Min
Zhang
,
Stephen P.
Collins
,
Alessandro
Bombardi
,
Peng
Li
,
Christoph
Rau
,
Marcus
Newton
Diamond Proposal Number(s):
[31929, 34075, 34025, 29880, 27621]
Open Access
Abstract: Although the LiCoO2 (LCO) cathode material has been widely used in commercial lithium ion batteries (LIB) and shows high stability, LIB’s improvements have several challenges that still need to be overcome. In this paper, we have studied the in-operando structural properties of LCO within battery cells using Bragg Coherent X-ray Diffraction Imaging to identify ways to optimise the LCO batteries’ cycling. We have successfully reconstructed the X-ray scattering phase variation (a fingerprint of atomic displacement) within a ≈ (1.6 × 1.4 × 1.3) μm3 LCO nanocrystal across a charge/discharge cycle. Reconstructions indicate strained domains forming, expanding, and fragmenting near the surface of the nanocrystal during charging, with a determined maximum relative lattice displacements of 0.467 Å. While discharging, all domains replicate in reverse the effects observed from the charging states, but with a lower maximum relative lattice displacements of 0.226 Å. These findings show the inefficiency-increasing domain dynamics within LCO lattices during cycling.
|
Oct 2024
|
|
