B07-B1-Versatile Soft X-ray beamline: High Throughput ES1
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Guangmeimei
Yang
,
Wei
Huang
,
Yifeng
Wang
,
Caiwu
Liang
,
Yuxiang
Zhou
,
Santosh
Kumar
,
Pilar
Ferrer Escorihuela
,
Parnia
Navabpour
,
Giuseppe
Sanzone
,
Trevor
Ferris
,
Georg
Held
,
Mark
Turner
,
Sarah J.
Haigh
,
Caterina
Ducati
,
Andreas
Kafizas
,
Reshma
Rao
Diamond Proposal Number(s):
[37550]
Open Access
Abstract: The scarcity of Ir presents a major challenge for scaling up its use as a water oxidation electrocatalyst in proton exchange membrane (PEM) water electrolysers. Developing conductive and stable supports is an effective way to reduce iridium loading while maintaining performance. However, the influence of support conductivity and stability on Ir-based catalytic activity remains poorly understood. The behaviour of the support is often obscured in conventional membrane electrode assembly (MEA) systems because IrOx itself is both highly conductive and exceptionally stable. To decouple support conductivity and passivation effects from the intrinsic conductivity of IrOx, we demonstrate a screening platform by studying a series of Ti-Nb alloy thin films produced by sputter deposition and investigate their performance as supports for IrOx water oxidation electrocatalysts. A range of electrochemical tests including accelerated stress tests (AST) were carried out on these samples, where characterisation techniques, including X-ray absorption spectroscopy (XAS), X-ray photoelectron spectroscopy (XPS) and high resolution transmission electron microscopy (HRTEM), demonstrated the in situ formation of passivation layers on these supports during water oxidation. Our results suggest that a ~10 nm oxide passivation layer forms on metallic Ti-based supports. On alloying Nb with Ti metal, a more insulating rutile TiO2 phase forms during water oxidation whereas an anatase TiO2, with higher conductivity, is observed on the pure Ti support. Consequently, although alloying Ti with Nb improves the bulk conductivity, the structure of the oxide passivation layer results in a drastic decrease of conductivity and water oxidation activity. Our results demonstrate the importance of the structure and composition of surface oxide phases formed during water oxidation in controlling the overall stability and conductivity of support materials.
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Apr 2026
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B07-B1-Versatile Soft X-ray beamline: High Throughput ES1
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Weiye
Ma
,
Lun
Zhang
,
Guanghan
Zhu
,
Hongrui
Kang
,
Haiyang
Yuan
,
Yongyi
Long
,
Zhiyi
Pan
,
Zhiqiang
Liu
,
Xiaojing
Liu
,
Jin
Liang
,
Yuxin
Liang
,
Zhenduo
Cui
,
Shengli
Zhu
,
Ying
Zhao
,
Zhonghui
Gao
Diamond Proposal Number(s):
[38100]
Open Access
Abstract: Poly(ethylene oxide) (PEO)-based electrolytes are promising for all-solid-state batteries but are typically limited to elevated temperatures due to PEO crystallinity and strong Li⁺–EO coordination. Here, we report a homogeneous PEO–LiTFSI electrolyte incorporating optimized Li3InCl6 that suppresses PEO crystallization, weakens Li⁺–TFSI⁻ coordination, and enhances Li-ion transport after acetonitrile solvent removal. This effect originates from the structural collapse of Li3InCl6 in acetonitrile, which exposes In3⁺ sites that preferentially adsorb TFSI⁻ anions, thereby disrupting the regular arrangement of PEO chains and inducing amorphization. In contrast to other oxide-based inorganic fillers, our results also found that the interface between PEO and Li3InCl6 enables efficient Li-ion transport. The resulting electrolyte achieves a high room-temperature ionic conductivity of 1.13×10⁻4 S cm-1 and excellent cycling stability with a LiNi0.8Co0.1Mn0.1O2 cathode, retaining 74 % capacity after 100 cycles at 0.3 C and 25 oC. To confirm the generality of this strategy and mechanism, we extended it to InCl3 and GaCl3 fillers, which similarly promoted amorphization in PEO–LiTFSI electrolytes. This work provides a general strategy to design amorphous polymer electrolytes for high-voltage solid-state batteries operating at room temperature.
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Apr 2026
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B18-Core EXAFS
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Diamond Proposal Number(s):
[14239]
Open Access
Abstract: Ni-rich layered oxides such as (LiNixMnyCo1−x−yO2 (x ≥ 0.6)) exhibit structural degradation, surface instability, and poor lithium ion transport, particularly under extreme temperature conditions, limiting their viability for next generation high energy batteries. This work demonstrates that low-level boron (B25) and tin–boron codoping (SB25) enhance the structural resilience and electrochemical performance of LiNi0.9Mn0.05Co0.05O2 (NMC955) cathodes across a range of temperatures: −5 °C, 25 °C, and 45 °C. Both dopants integrate into the layered α-NaFeO2 structure, expanding lattice parameters and reducing cation mixing, while preserving particle morphology. At sub-ambient temperatures (−5 °C) where slow Li-ion transport is the primary limitation, Sn–B codoping delivers a 25% improvement in specific capacity at 500 mA g−1 relative to pristine NMC955, suppresses the emergence of a second high resistance charge transfer (RCT reduces from 717 Ω to 71.4 Ω), and maintains the highest exchange current densities, 0.3 A m−2. At 25 °C RCT is reduced, from 10.34 Ω in pristine NMC955 to 8.79 Ω, and the effective diffusion coefficient increases, from 1.5 to 1.6 × 10−12 cm−2 s−1, demonstrating enhanced low temperature transport kinetics. Long-term cycling at approximately 1C shows improved capacity retentions of 92.7% (B25) and 88.7% (SB25) after 100 cycles versus 78% for undoped NMC. Postmortem XPS/XAS confirm that codoping suppresses electrolyte-induced transition metal fluorination and CEI thickening, with Sn–B showing the smallest change in Ni oxidation state and local coordination after 200 cycles. Together, these results establish Sn–B co-doping as a scalable and effective strategy to simultaneously enhance the structural stability, interfacial chemistry, and low-temperature transport kinetics of Ni-rich NMC cathodes for demanding lithium-ion battery applications.
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Apr 2026
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I15-1-X-ray Pair Distribution Function (XPDF)
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Diamond Proposal Number(s):
[30870]
Abstract: Electrochemical flash sintering (EFS) is a newly developed, solvent-free technique for ultrafast (∼2 s) densification of lithium-containing solid-state battery materials. Unlike conventional flash sintering—which relies on uncontrolled thermal runaway and requires high electronic conductivity—EFS couples electronic conduction in mixed conductors with Li+ transport across interfaces with pure ionic conductors in composite or multilayer architectures. Using spatially resolved synchrotron total scattering and pair distribution function analysis, we elucidate the mechanisms of EFS, contrasting them with conventional flash sintering of single-phase materials. Under conventional conditions, Li3V2(PO4)3 (LVP) undergoes localized decomposition and cracking at low frequencies and high currents, while Li1.3Al0.3Ti1.7(PO4)3 (LATP) requires high frequencies to overcome blocking behavior—resulting in electrode melting, infiltration, and vitreous extrusion at the pellet perimeter. In contrast, EFS enables densification of LVP–LATP composites at lower frequencies that fail for either phase alone, with reactions confined to localized hotspots. In an LVP–LATP|LATP|LVP–LATP multilayer, decomposition products are more broadly distributed, including vanadium migration into the electrolyte; nonetheless, no preferential cracking or new phases were observed at electrode–electrolyte interfaces. These findings establish EFS as a viable one-step processing strategy for integrating (electro)chemically distinct phases and lay the groundwork for its broader adoption in the dry fabrication of solid-state electrochemical energy storage systems.
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Apr 2026
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E02-JEM ARM 300CF
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Elif
Tezel
,
Beatrice
Garetto
,
Davide
Salusso
,
Dag K.
Sannes
,
Izar
Capel Berdiell
,
Sahra
Ahmed
,
Prantik
Sarkar
,
Stian
Svelle
,
Michael
Hirscher
,
Unni
Olsbye
,
Elisa
Borfecchia
,
Petra Ágota
Szilágyi
Diamond Proposal Number(s):
[41108]
Open Access
Abstract: This study investigates the catalytic performance of palladium nanoparticles supported on UiO-67, a zirconium-based metal–organic framework (MOF), for CO2 hydrogenation to methanol, emphasising the influence of the size and location of Pd particles in relation to the MOF matrix. Depending on the synthesis conditions, Pd particles were either supported on the outer surface of the MOF, forming larger nanoparticles (∼11–18 nm), or embedded within the MOF pores as smaller particles (∼1 nm), with their size constrained by the host framework. Advanced characterisation techniques, including X-ray diffraction (XRD), X-ray absorption spectroscopy (XAS), and transmission electron microscopy (TEM), coupled with catalytic testing, revealed that Pd clusters embedded within the MOF exhibited higher CO2 conversion and methanol selectivity. This superior performance is attributed not only to the increased surface area-to-volume ratio of the smaller Pd clusters, but also to the enlarged metal–MOF interface, which promotes favourable electronic interactions and enhances the accessibility of active sites. Notably, the confined Pd clusters suppressed methane formation, producing CO as the sole by-product. Despite local distortions at elevated temperatures, the UiO-67 framework maintained its structural integrity under reaction conditions, highlighting its thermal and chemical robustness. These findings deepen the understanding of structure–activity relationships in MOF-based catalysts and underscore the critical role of precise control over metal dispersion and metal-support interfaces in optimising catalytic efficiency and selectivity for CO2 hydrogenation.
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Mar 2026
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labSAXS-Offline SAXS and Sample Environment Development
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Diamond Proposal Number(s):
[40382]
Open Access
Abstract: The vast majority of small-molecule active pharmaceutical ingredients (APIs) are formulated in the crystalline state, for reasons including thermodynamic stability, ease of purification and characterisation, and better control over polymorphism. However, the selective crystallisation of polymorphic APIs provides a significant hurdle to overcome, especially in the case of API co-crystals. Herein we report a series of low-molecular-weight organogels (LMWGs) which can be used to selectively crystallise APIs. In solution, these LMWGs (2–10 mg mL−1) self-assemble through hydrogen bonding to form stable gels which feature nano-structured morphologies. When utilised as crystallisation media, these LMWGs can influence crystal growth, as evidenced by the discovery of two novel 1[thin space (1/6-em)]:[thin space (1/6-em)]1 co-crystals of chlorzoxazone with nicotinamide and chlorzoxazone with isonicotinamide. This work highlights the potential of LMWGs as another means of controlling API crystallisation.
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Mar 2026
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I15-1-X-ray Pair Distribution Function (XPDF)
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Diamond Proposal Number(s):
[37504]
Open Access
Abstract: Crystalline hybrid organic–inorganic structures from the coordination polymer (CP)/metal–organic framework (MOF) family have recently emerged as materials which liquify upon heating to high temperature and then transform into glass upon cooling to room temperature. This melt-quench process of this material family generally requires an anaerobic atmosphere to avoid oxidation of organic component at high temperature. Anaerobicity here brings in an extra cost and makes melt-quench setup robust. Besides, these hybrid liquids often show intriguing thermal behaviour such as exothermic recrystallization (on cooling), cold crystallization (on reheating), etc. which again limits the typical melt-quench process of glass fabrication and processability. Here we turn to hybrid organic–inorganic structures of one-dimensional (1-D) family and design five 1-D (PrPh3P)2[M(dca)4] (PrPh3P = propyltriphenylphosphonium; M = Mn, Fe, Co, Ni, Cu; dca = dicyanamide) compounds which overcome above hurdles and were successfully vitrified upon direct in-situ melt-quenching on laboratory time scales under aerobic conditions. The combined spectroscopic and X-ray total scattering studies reveal successful structural characterization of these glasses that largely retain the coordination bonding of the crystalline phase and show valuable physical properties such as low liquid fragility (m), large ‘glass-crystal network density deficit’ (Δρ/ρg)network, high glass-forming ability (GFA) and polymer-like mechanical hardness (H).
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Mar 2026
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I11-High Resolution Powder Diffraction
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Brinda
Kuthanazhi
,
Debalina
Banerjee
,
Dmitry
Maslennikov
,
Andrij
Vasylenko
,
Jan P.
Scheifers
,
Cara J.
Hawkins
,
Daniel
Ritchie
,
Craig M.
Robertson
,
Marco
Zanella
,
Troy D.
Manning
,
Luke M.
Daniels
,
Marina R.
Filip
,
Matthew S.
Dyer
,
Laura M.
Herz
,
John B.
Claridge
,
Matthew J.
Rosseinsky
Diamond Proposal Number(s):
[37989]
Open Access
Abstract: We explore multiple-cation chalco–halide phase fields evaluated by their synthetic accessibility using machine learning models. Exploratory synthesis guided by computational tools leads to the discovery of two new compounds; CuSn2SI3 and Cu0.35Sn5.29S2I7, their structures, and electronic and optical properties are reported herein. This is the first report of a stable quaternary compound in the Cu–Sn–S–I phase field. The two new compounds show related crystal structures where Sn4S2I4 layers are a common structural motif in both. These Sn4S2I4 layers are connected by Cu2I2 layers and disordered Cu–Sn–I layers, forming the three-dimensional structures of CuSn2SI3 and Cu0.35Sn5.29S2I7 respectively. Electronic band structure calculations using density functional theory show the presence of a direct band gap in CuSn2SI3 and suggest anisotropic transport, in line with the layered structure of the compound. A mixture of the two compounds with ∼86% CuSn2SI3, shows a band gap in the visible region, close to 2.1 eV and a significant photo-induced charge carrier mobility of ∼1.3 cm2 V−1 s−1. This demonstrates Cu–Sn chalco–halides can form a promising phase space to explore for solar absorber materials, with further design and tuning of band gap.
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Mar 2026
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I15-1-X-ray Pair Distribution Function (XPDF)
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Emily V.
Shaw
,
Javier
Pérez-Carvajal
,
Elena
López-Elvira
,
Shaoliang
Guan
,
Timothy
Lambden
,
Georgina P.
Robertson
,
Arad
Lang
,
Joonatan E. M.
Laulainen
,
Celia
Chen
,
Chumei
Ye
,
Anna
Herlihy
,
Catherine
Dejoie
,
David A.
Keen
,
Paul
Midgley
,
Thomas D.
Bennett
,
Celia
Castillo-Blas
Diamond Proposal Number(s):
[31401, 39316]
Open Access
Abstract: We report a scalable, water-based methodology for the direct room-temperature synthesis of porous amorphous UiO-66-type metal–organic frameworks (aMOFs), enabling the incorporation of a range of functionalised terepthalate linkers without organic solvents during framework formation. Powder X-ray diffraction and scanning electron diffraction confirm the formation of truly topologically amorphous UiO-66 derivatives, while pair distribution function (PDF) analysis shows that the amorphous frameworks retain the local structural motifs of their crystalline analogues despite the loss of long-range order. Relative to crystalline UiO-66, the directly synthesised amorphous UiO-66 exhibits a reduced but permanent porosity (BET surface area 286 vs. 997 m2 g−1 CO2-accessible pore volume 0.196 vs. 0.519 cm3 g−1), together with a high concentration of defects, consistent with a cluster[thin space (1/6-em)]:[thin space (1/6-em)]linker ratio of 1[thin space (1/6-em)]:[thin space (1/6-em)]5.3 compared with 1[thin space (1/6-em)]:[thin space (1/6-em)]6 for the ideal crystalline framework. In the esterification of levulinic acid, amorphous UiO-66 reaches 87.7% conversion to methyl levulinate after 3 h, compared with 75.5% for crystalline UiO-66, and retains 95% of its initial activity after five catalytic cycles (vs. 86% for the crystalline analogue). These results demonstrate that direct, water-based synthesis provides access to functional, porous, and highly defective amorphous UiO-66 materials with catalytic performance comparable to or exceeding that of their crystalline counterparts under the conditions studied.
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Mar 2026
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B21-High Throughput SAXS
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Open Access
Abstract: The fabrication of superlattices is nontrivial because nanoparticles are notoriously difficult to employ due to the complex nanoscale forces among them. An effective way to manipulate these nanoscale forces is to use a soft corona around the solid core. The soft corona can be engineered to alter the forces between nanoparticles—either attracting or repelling them, and thereby influence their self-assembly process. Here, a deep analysis is proposed on how amines of different lengths (C8 to C18) can influence the hierarchical superlattice organization of cerium oxide nanoparticles, from both structural and energetic perspectives, and the consequent optical properties. The aim is to demonstrate how it is possible to shift from disordered to ordered aggregates and how to obtain one structure instead of another by modulating the geometrical and energetic parameters of soft corona/solid core nanoparticles. The results show that organic coating plays a key role in the self-aggregation process of superlattices with advanced optical properties, thereby broadening the range of potential applications for nanoparticles.
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Feb 2026
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