I12-JEEP: Joint Engineering, Environmental and Processing
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Emily C.
Giles
,
Abbey
Jarvis
,
Pierrot S.
Attidekou
,
Kieran
O'Regan
,
Rosie
Madge
,
Alexander T.
Sargent
,
Beatrice
Browning
,
Anton
Zorin
,
Roberto
Sommerville
,
Alex J.
Green
,
Stefan
Michalik
,
Philip A.
Chater
,
Daniel
Reed
,
Emma
Kendrick
,
Laura L.
Driscoll
,
Peter
Slater
,
Phoebe K.
Allan
,
Paul
Anderson
,
Luke
Sweeney
Open Access
Abstract: Understanding the degradation of large format lithium-ion pouch cells – critical for electric vehicle applications – is vital to extend their lifetime and allow potential second-life application. Here, the impact on capacity fade and material degradation in two end-of-life cells, which were additionally subjected to accelerated aging to mimic extended use in second-life applications, were examined using powder synchrotron X-ray diffraction, Raman spectroscopy and electrochemical impedance spectroscopy, complemented by detailed post mortem analyses. The dominant mechanism of capacity loss under these conditions was found to be lithium inventory depletion, driven by processes such as electrolyte decomposition, lithium plating and solid electrolyte interphase growth. Structural changes in the graphite anode, including amorphization and reduced active material, were more pronounced under severe overcharging conditions. The blended cathode showed lithium inventory loss in both phases, but 92–94% capacity recovery was observed on subsequent cycling in half cells vs Li, illustrating its robustness, with little structural degradation observed. The finding that electrolyte degradation/loss in these cells was a more critical contributor to cell degradation toward the knee-point than electrode active material degradation/loss indicates that increasing – or replenishing – the electrolyte content could be a strategy to extend the usable life of such cells.
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Nov 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[14657]
Open Access
Abstract: Learning to control reaction kinetics is essential for translating any chemical technology into real-world application. Based on time-resolved in situ powder X-ray diffraction data, we demonstrate the opportunity to tune mechanochemical reaction rates through the pre-activation of the starting reagents. For three model co-crystal systems, the pre-activation of the most stable reagent yields up to a ca 10-fold increase in the reaction rate, whilst negligible kinetic enhancement is seen when the less stable reagent is pre-activated. Moreover, we demonstrate how the polymorphic outcome of mechano-co-crystallization is also sensitive to pre-activation of the starting material. Our results suggest that reproducibility of mechanochemical processes requires detailed understanding over the origin and history of reagent powders, whilst providing a new conceptual framework to design and control mechanochemical reactions.
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Nov 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[35888]
Open Access
Abstract: Understanding the mechanistic interplay between phase transformation and grain fragmentation is critical for microstructural control in advanced structural steels subjected to severe shear. Here, we investigate the activation sequence of retained-austenite transformation and grain fragmentation along the radial strain gradient of a single QP1180 steel disk processed by high-pressure torsion. Synchrotron-based high-energy X-ray diffraction and microscopy reveal a pronounced austenite (γ) → martensite (α′/α) transformation that saturates at a critical equivalent von Mises strain
∼ 8.5. Concomitantly, γ grain size decreases sharply up to
, while γ peak broadening and microstructural analysis suggest limited grain fragmentation of austenite during transformation. These findings demonstrate that γ-phase reduction is primarily driven by phase transformation prior to the onset of defect-induced fragmentation. This mechanistic activation order and the critical strain
provide key inputs for calibrating physics-based constitutive models and defining robust process windows for industrial forming operations and component design.
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Oct 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[30281]
Open Access
Abstract: Ti-6Al-4V (Ti-64) is one of the most widely used α + β titanium alloys. During its thermomechanical processing, strong and heterogeneous crystallographic textures can develop that are detrimental to mechanical performance. Existing texture data for Ti-64 in the α + β regime is limited and lacks detail on how the texture of both the hexagonal close-packed (HCP) α and body-centred cubic (BCC) β phases evolve during hot deformation. In this study, a comprehensive dataset of α and β textures was generated from hot rolling experiments at nine temperatures (825–1020 °C) and three rolling reductions (up to 87.5 pct), with different starting microstructures. High-throughput electron backscatter diffraction and synchrotron X-ray diffraction were used to characterise texture development. Results show that a moderate 0002//TD α alignment forms at all subtransus temperatures and becomes dominant above 895 °C, increasing with both strain and temperature. In contrast, the β texture remains weak at lower temperatures but develops a strong rotated cube component near and above the β-transus. Lamellar-starting microstructures led to slightly stronger textures but similar texture components. The full dataset has been made publicly available to support future modelling efforts and improve understanding of dual-phase texture development in titanium alloys.
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Aug 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Ilaria
Quaratesi
,
Ioan
Călinescu
,
Petre
Chipurici
,
Elisa-Gabriela
Dumbravă
,
Andrei
Cucos
,
Mohamed Yassine
Zaki
,
Pellegrino
La Manna
,
Adrian
Bercea
,
Miruna Silvia
Stan
,
Stefan
Michalik
,
Chloe
Pearce
,
Marianne
Odlyha
,
Genoveva
Burca
,
Elena
Badea
Diamond Proposal Number(s):
[35634]
Open Access
Abstract: This study presents an ultrasound-assisted synthesis of β-cyclodextrin/hydroxyapatite composites to be used as green and safe auxiliaries in the tanning process. A combination of spectroscopic and non-spectroscopic techniques such as DLS (dynamic light scattering), ZP (zeta potential), XRD (X-ray diffraction), SEM (scanning electron microscopy) and ATR-FTIR (attenuated total reflectance-Fourier transform infrared spectroscopy) were used to thoroughly characterize the eight composites obtained by varying the ultrasound process parameters. While not cytotoxic, all composites had strong antibacterial action against Brevibacterium lines, Staphylococcus aureus, Escherichia coli, and Staphylococcus epidermis. All composites underwent lab-scale tanning tests, but only those exhibiting the most suitable set of tanning abilities underwent pilot-scale testing. The composites' interaction with the collagen matrix was assessed by micro-DSC (micro-differential scanning calorimetry), TG/DTG/DTA (thermal analysis), 1H unilateral NMR (proton nuclear magnetic resonance), ATR-FTIR, in-situ temperature synchrotron-based XRD and standard tests (UNI EN ISO 3380: 2015, UNI EN ISO 2589: 2016, UNI EN ISO 105- B02:2014). Thermal stability, dye penetration, thickness, colour fastness, surface appearance and microbiological protection were all improved for the leather treated with a small amount of composite added to the wet finish float. These findings demonstrate the benefits of β-cyclodextrin/hydroxyapatite composites as safe and sustainable tanning additives.
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Apr 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[37256]
Open Access
Abstract: he high brilliance and coherence of light generated at synchrotron facilities make synchrotron X-ray imaging an invaluable tool for the non-destructive analysis of samples across a range of interdisciplinary sciences. For samples with low attenuation contrast, phase-contrast imaging and phase-retrieval techniques can be used to enhance image contrast and provide complementary phase-shift information. In this work, we demonstrate the phase-contrast imaging capabilities of the Diamond Light Source I12-JEEP beamline using two samples: a fly encased in 4 mm of steel, and a lower chicken leg (drumstick) bones with surrounding soft tissue. Techniques such as X-ray phase-contrast imaging, near-field speckle-based phase-contrast tomography and propagation-based (in-line) phase-contrast tomography are investigated; additionally, the effects of propagation distance, speckle mask material, number of speckle positions, and phase-retrieval algorithm on the quality of radiographic images and reconstructed tomography volumes are compared. The experimental setup, data acquisition settings, as well as phase retrieval and tomography reconstruction parameters are detailed, and concluding remarks are made regarding the strengths and weaknesses of each technique, their use case, and how the data acquisition parameters can be optimised for an extended field-of-view or in-situ imaging setup available at I12.
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Jan 2025
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B18-Core EXAFS
I11-High Resolution Powder Diffraction
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Prathmesh
Bhadane
,
Dhruv
Menon
,
Prateek
Goyal
,
Mohammad Reza
Alizadeh Kiapi
,
Biraj
Kanta Satpathy
,
Arianna
Lanza
,
Iuliia
Mikulska
,
Rebecca
Scatena
,
Stefan
Michalik
,
Priya
Mahato
,
Mehrdad
Asgari
,
Xu
Chen
,
Swaroop
Chakraborty
,
Abhijit
Mishra
,
Iseult
Lynch
,
David
Fairen-Jimenez
,
Superb K.
Misra
Diamond Proposal Number(s):
[39677, 38403]
Abstract: Recycling and recovery of rare earth elements (REEs) from electronic wastes can accelerate efforts to mitigate the environmental burden associated with their excessive mining, while catering for their growing demand. Contemporary recovery strategies are yet to make an impact at an industrial scale due to low REE uptakes, complex mechanisms, and high regeneration energies, leading to an overall poor scalability. Here, we report a two-dimensional metal–organic framework (BNMG-1) featuring a dense arrangement of active adsorption sites for the high uptake of heavy and light REEs. BNMG-1 with a lateral dimension of ca. 350 nm and a thickness of 14 nm was synthesized via a facile one-pot reaction using a green solvent under room temperature and atmospheric pressure. The two-dimensional structure of BNMG-1 was resolved using three-dimensional electron diffraction and EXAFS analysis. Batch experiments showed BNMG-1 to have an adsorption capacity of 355.8 mg/g for Nd3+, 323.1 mg/g for Y3+, 331 mg/g for Dy3+, 329mg/g for Tb3+ and 333 mg/g for Eu3+, which is a near-benchmark performance for a non-functionalised MOF. The adsorption efficiency for Nd3+ reached 99 % by 6 h and 88 % by 48 h for Y3+. The adsorption efficiency did not get affected over a pH range of 3 to 6 and retained > 99 % of its adsorption capacity for up to 4 cycles. For application on real-life samples, CFL lamp waste and waste magnets were used as a reservoir of heavy (Yttrium) and light (Neodymium) REEs. BNMG-1 demonstrates an efficient recovery of 57 % for Neodymium from scrap magnets and 27 % for Yttrium from waste fluorescent lamps. This performance, which is maintained under acidic conditions and over multiple cycles, highlights the competitiveness of BNMG-1 for the economic large-scale recovery of REEs.
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Dec 2024
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I15-1-X-ray Pair Distribution Function (XPDF)
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Diamond Proposal Number(s):
[20770]
Abstract: The structure of evaporated amorphous GexSbxTe100−2x (x = 6, 9, 13) alloys was investigated by neutron diffraction, X-ray diffraction, and extended X-ray absorption spectroscopy at the Ge, Sb, and Te K-edges. Large-scale structural models were generated by fitting the experimental datasets (five for each composition) simultaneously in the framework of the reverse Monte Carlo simulation technique. It was found that the alloys are chemically ordered (Ge and Sb have predominantly Te neighbors) and within the experimental uncertainty, each component satisfies the 8 – N rule. A comparison with the pair correlation functions of melt-quenched Ge20Te80 revealed that the first minimum of gTeTe(r) is shallower in the ternary alloys than in Ge20Te80. On the other hand, the separation of the first and second coordination environments of Ge atoms is stronger in the Ge–Sb–Te alloys investigated.
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Nov 2024
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Open Access
Abstract: Short range order of a ternary Mg82Ca8Au10 biodegradable amorphous alloy was studied by combining diffraction datasets and Au L3 edge EXAFS data by the Reverse Monte Carlo simulation technique. It was found that while the Mg–Mg bond length agrees well with the empirical atomic diameter of Mg, both the Mg–Ca and Mg–Au mean interatomic distances are ∼9 % shorter than the sum of the corresponding atomic radii. The Ca–Au bond length exhibits ∼14 % shortening. The linear expansion coefficients of the glass determined from the temperature induced shift of the first peak of the structure factor and the reduced pair distribution function are ∼3.7 × 10−5 K−1 and ∼3.1 × 10−5 K−1, respectively. During devitrification, two crystalline phases emerge from the amorphous alloy: hexagonal AuMg3 and the solid solution of Ca in hexagonal close packed Mg. The thermal expansion behaviour of the AuMg3 unit cell was also determined using diffraction data.
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Oct 2024
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[34953]
Open Access
Abstract: We use in situ synchrotron X-ray diffraction measurements to monitor the solvothermal crystallization mechanism of the aperiodic metal–organic framework TRUMOF-1. Following an initial incubation period, TRUMOF-1 forms as a metastable intermediate that subsequently transforms into an ordered product with triclinic crystal symmetry. We determine the structure of this ordered phase, which we call msw-TRUMOF-1, and show that it is related to TRUMOF-1 through topotactic reorganization of linker occupancies. Our results imply that the connectivity of TRUMOF-1 can be reorganized, as required for data storage and manipulation applications.
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Sep 2024
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