I12-JEEP: Joint Engineering, Environmental and Processing
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Evangelia
Tsolaki
,
Alexandra
Howard
,
Yunze
Jiang
,
Xingyu
Lu
,
Luyao
Wang
,
Amjad
Abouselo
,
Oxana V.
Magdysyuk
,
Thomas
Zillhardt
,
Dejan-Kresimir
Bucar
,
Jonathan C.
Burley
,
Gareth R.
Williams
,
James
Mccabe
Diamond Proposal Number(s):
[36356]
Open Access
Abstract: The development of eutectic-based amorphous solid dispersions (ASDs) is often constrained by the time and material required to identify suitable drug–coformer combinations. Here, we present a miniaturised high-throughput workflow that integrates picolitre-volume 2D inkjet printing, predictive thermodynamic modelling, and scalable processing to accelerate eutectic formulation design for the model API nifedipine. Binary systems were printed as microarrays and screened microscopically, enabling rapid identification of promising eutectic pairs using minimal material. The Schroeder–Van Laar equation was applied to predict eutectic compositions and onset temperatures, which were subsequently validated through scale-up and full phase-diagram construction. Selected formulations were then processed by hot-melt extrusion to generate amorphous solid dispersions. This end-to-end strategy, spanning ultrafast microarray screening to continuous manufacturing, provides a robust and material-efficient platform for eutectic-based ASD development and substantially shortens formulation timelines for poorly soluble APIs such as nifedipine.
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Aug 2026
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B18-Core EXAFS
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Diamond Proposal Number(s):
[37961]
Open Access
Abstract: In the present work, we report the exsolution of CoFe nanoalloy nanoparticles from Co and Fe co-doped lanthanum aluminate perovskite oxide, LaAl0.90Co0.05Fe0.05O3, and assess the perovskite oxide as an oxygen reduction reaction (ORR) electrocatalyst. We optimized both intrinsic and extrinsic material properties of perovskites to achieve good electrocatalytic performance in the kinetic and mass-transfer controlled region. Firstly, we demonstrated that the near surface segregation of B-site cation (Co) under reducing environment at low temperature (at 500 °C), believed to represent the initial stage of exsolution, led to high ORR activity in the mass-controlled region, with specific and mass activities of 4.9 mA/cm2 and 37.5 A/g (@0.4 V versus RHE), respectively. Secondly, reducing the particle size of perovskite oxide increased surface exposure to the reducing environment promoting the CoFe nanoalloy particle exsolution. The results demonstrate that cation enrichment in subsurface region, near grain boundaries contributes more effectively to ORR activity than exsolution in the form of nanoparticles in this perovskite oxide composition. Nevertheless, achieving fast charge transfer-kinetics without the use of precious metals still remains a challenge with lanthanum aluminates, as indicated by onset potentials of 0.84 V and 0.81 V (versus RHE) for the pristine and reduced perovskite oxide, respectively. Notably, impregnation of perovskite oxide with 0.2 wt. % Pt followed by heat treatment in reducing atmosphere at 500 °C increased the onset potential to 0.9 V. Overall, this study suggests that non-precious metal-doped lanthanum aluminate, LaAl0.90Co0.05Fe0.05O3, exhibits strong electrocatalytic activity and is further enhanced through impregnation treatment.
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Jun 2026
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I11-High Resolution Powder Diffraction
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Diamond Proposal Number(s):
[38160]
Open Access
Abstract: Zn-substituted Na0.75Mn0.68Ni0.25Zn0.07O2 has been synthesized in P3, P2, and composite P2/P3 structures and compared with unsubstituted Na0.7Mn0.75Ni0.25O2 analogues as positive electrodes for sodium-ion batteries. The synthesis temperature was shown to provide a means of controlling the phase ratio of P2 and P3 phases. Powder diffraction measurements, high-resolution transmission electron microscopy (TEM), and selected area electron diffraction (SAED) revealed that Zn substitution enhanced the ordering of the transition metal (TM) layers. Electrochemical studies combined with XAS measurements showed that after Zn substitution, Ni activity was enhanced, while the irreversible activity of O and Mn was suppressed. Structural transformations were suppressed, and the reversibility of Zn-substituted samples on cycling was improved. Among the Zn-substituted samples, Zn–P2/P3 delivers the best electrochemical performance with an initial capacity of 121 mAh g–1 at a rate of 25 mA g–1 and 90% capacity retention after 100 cycles in half-cells. This work reveals the intrinsic correlation among cation doping, synthesis conditions, and crystal phase compositions but also provides a reliable strategy for designing high-stability composite layered cathode materials for sodium-ion batteries.
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Jun 2026
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[30778]
Open Access
Abstract: The thermo-mechanical response of reduced activation ferritic martensitic steel EUROFER97 is governed by dislocation-mediated deformation processes, which are critical for designing and predicting structural behavior under fusion-relevant loading conditions. In this study, the deformation behavior of batch-2 EUROFER97 is investigated using in-situ high energy synchrotron X-ray diffraction during monotonic tensile testing from room temperature to elevated temperature (nominal 500°C, corresponding to a measured value of 460°C) and asymmetric cyclic tensile loading at 460°C. Monotonic tensile tests are used to establish baseline temperature-dependent evolution of dislocation character and density. The primary focus is on asymmetric cyclic tensile loading, representative of ratcheting conditions, during which cycle-resolved analysis of dislocation recovery is realized. Diffraction line profile analysis is employed to quantify total dislocation density and the relative contributions of edge and screw components. The experimental data are interpreted using physically based recovery models, allowing extraction of activation energies and volumes associated with character-specific dislocation recovery. The results show that, while the overall deformation behavior is consistent with previously reported trends in EUROFER97 and related steels, the present work provides quantitative characterization of recovery parameters under non-fully reversed cyclic loading. These parameters offer physically meaningful input for dislocation-based constitutive models describing cyclic plasticity and ratcheting. The findings support the transferability of micromechanical deformation behavior across industrial batches, while emphasizing the importance of dislocation kinetics in designing and modelling fusion structural materials under thermo-mechanical loading.
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Apr 2026
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I15-1-X-ray Pair Distribution Function (XPDF)
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Maximillian G.
Stanzione
,
Oxana V.
Magdysyuk
,
Daniel J. M.
Irving
,
Chinnasamy
Murugesan
,
Nicole L.
Kelly
,
Yingling
Liao
,
Pech
Thongkam
,
Heitor S.
Seleghini
,
Paul S.
Wheatley
,
David B.
Cordes
,
Simon J.
Coles
,
Daniel N.
Rainer
,
Aamod V.
Desai
,
Sharon E.
Ashbrook
,
Julia L.
Payne
,
Russell E.
Morris
,
A. Robert
Armstrong
Diamond Proposal Number(s):
[36333]
Open Access
Abstract: Organic anode materials for sodium-ion batteries are attracting a great deal of interest due to their sustainability and design flexibility. However, the Na+ insertion mechanism is poorly understood, especially for disordered organic anode materials. A lack of understanding restricts optimization efforts and potential commercialization. Herein, we apply a range of characterization techniques, such as three-dimensional electron diffraction, powder X-ray diffraction, Raman spectroscopy, electron paramagnetic resonance spectroscopy, and pair distribution function (PDF) analysis to a model system, sodium naphthalene-2,6-dicarboxylate, to elucidate the Na+ storage mechanism. A combined ab initio random structure search and PDF study was conducted to postulate a structure of sodiated Na2+xNDC (s-NDC). Our work reveals an expansion in the Na+–O storage layer to allow for the accommodation of inserted Na+. Meanwhile, the naphthalene units exist as radical species, promoting a reorientation to accommodate the inserted Na+, as well as facilitating a stabilizing π interaction. Ultimately, our results illustrate the efficacy of using a multi-technique approach to study the sodiation mechanism of an organic anode material and offer insight into the sodiated structure. This approach can inform the strategic molecular design of future organic anode materials.
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Mar 2026
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I12-JEEP: Joint Engineering, Environmental and Processing
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Open Access
Abstract: The preservation of archaeological bone is of great importance for both archaeological and conservation science studies. Traditional methods of preservation assessment, such as attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), are minimally invasive and destructive. Neutron and X-ray tomography offer a totally non-invasive novel analysis method for the state of preservation of archaeological bones. Seven archaeological animal bones were selected for analysis based on animal maturity, species, visual factors, and ATR-FTIR analysis results. Archaeological bone is a hierarchical composite material constructed from both organic and mineral components; therefore, neutron tomography and synchrotron X-ray tomography have been combined in this novel approach to assess the state of preservation of animal archaeological bone. The neutron data demonstrated that the organic distribution along the diaphysis of archaeological bones varied significantly both within bones and between different animal bones. There is minimal consistency between the samples, emphasizing the inhomogeneity in archaeological bone collections. X-ray tomography revealed unseen physical details, including cracks and substantial damage. The collection of this information via non-invasive methods is highly valuable for cultural heritage, providing a deeper understanding of the observed inhomogeneity in ATR-FTIR analysis data and revealing obscured physical details.
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Aug 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
I15-Extreme Conditions
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Diamond Proposal Number(s):
[21147, 19558]
Abstract: The strength-ductility trade-off in additively manufactured (AM) β Ti alloys remains a significant challenge. In this study, we employed a cost-effective in-situ alloying laser powder bed fusion approach with optimized processing parameters to fabricate a nearly fully dense, chemically homogeneous β Ti-12Mo alloy. We then examined how solution-treatment duration influences the tensile behavior of the AM Ti-12Mo alloy. The optimally solution-treated alloys exhibited high tensile yield strength (725–741 MPa) and commendable ductility (22–36 %) along both the 0° and 90° orientations relative to the build direction. Focusing on the underlying deformation mechanisms perpendicular to the build direction, we report a uniform elongation of 17.9 % and a pronounced strain hardening rate (∼2300 MPa at 4 %), which we elucidate via in-situ high-energy synchrotron X-ray diffraction and microstructural characterization. The high yield strength is primarily attributed to the presence of Mo-lean embryonic athermal ω nanoparticles. During plastic deformation, both twinning and phase transformation contribute to the high strain hardening rate. At the early stage (strain < 1.9 %), deformation is dominated by {332}< 113 >β twinning, whereas at later stages, the deformation-induced α'' phase becomes significant. The volume fraction of α'' phase increases with strain, supporting the continuous hardening. Notably, irrational {112}< 751 >β, secondary {112}< 111 >β, and {130}< 310 >α'' nano-twins confine the primary structures to nanograins and sustain strain hardening. This study sheds light on designing high-performance β Ti-12Mo alloy via AM followed by heat treatment.
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Jun 2025
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B18-Core EXAFS
I11-High Resolution Powder Diffraction
I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[9610, 12763, 9019, 32893, 11574]
Open Access
Abstract: Iron-based superconductors have attracted much attention for their high superconducting temperatures and high upper critical fields, which make them promising candidates for application as well as fundamentally important for our understanding of superconductivity. One feature of these superconductors is their ability to intercalate and deintercalate species from between their iron-containing layers, something not available in cuprate high-temperature superconductors or niobium-based conventional superconductors used in technologies. This provides an opportunity for switchable changes in the superconducting properties as a function of chemical conditions, but the resulting structures are often hard to characterize due to loss of crystallinity and sometimes the formation of multiphase products. Here, we explore both the synthesis and decomposition of potassium and ammonia-intercalated iron selenide superconductors through in situ powder X-ray diffraction. We report a complete phase diagram including two new solution-stable ammonia-rich phases and several metastable forms. We give accurate characterization of the reported ammonia-poor forms using a combination of neutron and X-ray powder diffraction, using an innovative supercell approach to describe the phase breadth within the samples. These results give rare insight into stepwise changes occurring in solids along multiple reaction pathways, which demonstrate the importance of in situ diffraction techniques.
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May 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[26767]
Open Access
Abstract: Lithium ion batteries are pivotal for clean energy storage and mitigating climate change. In this study, we employ operando synchrotron X-ray computed tomography to investigate the dynamic evolution of battery cathode microstructure. We focus on tracking changes in porosity and pore size distribution at the microscale and cathode thickness at the macroscale during the lithiation and delithiation processes within a commercially configured battery. Image quality was enhanced using both conventional image processing methods and a Super-Resolution Convolutional Neural Network (SRCNN) model. Our findings revealed a slight increase in the cathode solid volume fraction and specific surface area as the battery transitioned from its pristine state to fully lithiated, followed by a reduction during delithiation. This behavior was attributed to the expansion of the cathode material and phase transitions during lithiation, which split larger pores into smaller ones, as evidenced by the increase in surface area. Cathode thickness also exhibited expansion during lithiation and contraction during delithiation. These results offer valuable insights into the structural changes that contribute to battery aging, helping researchers better understand how these different parameters change over time. This understanding is crucial for designing more durable and sustainable batteries in the future, both in terms of specific design and material selection, to enhance resistance during charge and discharge cycles to improve performance and longevity.
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Apr 2025
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I12-JEEP: Joint Engineering, Environmental and Processing
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Abstract: The effect of substituting linkers with two additional methyl groups for conventional benzimidazolate on the thermal expansion behaviour of ZIF-62 was investigated by high-energy in situ X-ray diffraction. Increased structural integrity was observed with the addition of methyl groups, and variable anisotropic thermal expansion was discovered in ZIF-62 and its derivative.
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Oct 2024
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