B21-High Throughput SAXS
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Giuseppe Junior
Mosca
,
Simone
Russo
,
Valentina
Pelliccioli
,
Martina
Quaglia
,
Pietro
Pettinari
,
Alessandro
Cangiano
,
Diego
Colombo
,
Paola
Perego
,
Giovanni L.
Beretta
,
Laura
Morelli
,
Giuseppe
Vitiello
Diamond Proposal Number(s):
[34244]
Open Access
Abstract: Colloidal quantum dots (QDs) represent a versatile class of luminescent nanomaterials whose physicochemical and interfacial properties can be engineered for advanced bio-related applications. Herein, the wet-precipitation synthesis and surface engineering of ultra-small fluorine-doped ZnO quantum dots (F/ZnO QDs) were proposed and their formulation into stable amphiphilic nanosystems using synthetic glycoglycerolipids. To control aggregation and interfacial behavior, the QDs were first capped with oleylamine and subsequently functionalized through an emulsion-based approach with mono-acyl or di-acyl glycoglycerolipids, yielding double-coated amphiphilic nanoformulations. The resulting materials were extensively characterized by TEM, DLS, zeta-potential measurements, XRD, FTIR/ATR, UV–Vis, and fluorescence spectroscopy, allowing to explore correlations between surface chemistry, colloidal stability, and optical properties. Glycoglycerolipid functionalization led to a marked improvement in aqueous dispersibility and long-term colloidal stability while preserving the enhanced fluorescence induced by fluorine doping. Biological assays confirmed the cytocompatibility of the coated QDs and supported their suitability for further biointerface studies. This work highlights glycoglycerolipid-based amphiphilic coatings as an effective strategy to tailor the surface and colloidal properties of ZnO-based QDs, enabling the development of stable luminescent nanomaterials as biocompatible nanoprobes and for bio-interfacial applications.
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Aug 2026
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B22-Multimode InfraRed imaging And Microspectroscopy
I18-Microfocus Spectroscopy
labSAXS-Offline SAXS and Sample Environment Development
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Diamond Proposal Number(s):
[34998]
Open Access
Abstract: This study addresses the critical challenge associated with the removal of reactive yellow dyes from aqueous media and industrial wastewater streams. Owing to their pronounced chemical stability and resistance to conventional degradation techniques, such dyes constitute a substantial environmental concern. In this context, the present work investigates the efficacy of unmodified magnetite nanoparticles (plate-like rounded structures 6–23 nm in size), synthesised under rigorously controlled conditions and well characterised, as high-performance adsorbents for the sequestration of persistent dye species exhibiting limited susceptibility to rapid degradation. The effects of key operational parameters on dye removal efficiency were systematically evaluated to establish optimal treatment conditions. Complete removal of reactive yellow dye (100%) was achieved within 30 min at low initial dye concentrations (20 mg/L) under mildly acidic conditions and continuous agitation. Adsorption equilibrium studies, interpreted using the Langmuir isotherm model, revealed a maximum adsorption capacity of 33 mg/g under optimised conditions. Thermodynamic analysis indicated that the adsorption process is spontaneous (−ΔG° ≈ 46–54 kJ/mol) and endothermic (ΔH° = 21.12 kJ/mol), accompanied by an increase in system disorder (ΔS° = 0.2 kJ/mol × K). Importantly, experiments conducted using real wastewater matrices demonstrated performance comparable to that obtained in deionised water, thereby underscoring the practical applicability of the proposed system. Furthermore, the nanoparticles retained more than 90% removal efficiency after five consecutive adsorption–desorption cycles, employing a basic eluent for dye desorption and surface regeneration. The intrinsic magnetic properties of the adsorbent additionally enable facile recovery and potential reutilisation in secondary applications, including asphalt production. Collectively, these findings highlight the considerable potential of magnetite nanoparticles as effective and reusable adsorbents for wastewater remediation and support further investigation toward pilot-scale implementation.
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Jul 2026
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B21-High Throughput SAXS
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Bridget
Tang
,
Philip
Kitchen
,
Luke M.
Broadbent
,
Steven D.
Quinn
,
Nawal
Hassan
,
Siriporn
Chaimueangchuen
,
Barbara
Gerbelli
,
Katsuaki
Inoue
,
Nathan
Cowieson
,
Fátima
Herranz-Trillo
,
Alice J.
Rothnie
,
Roslyn M.
Bill
,
Paul D.
Topham
,
Alan D.
Goddard
,
Jacob J. K.
Kirkensgaard
,
Matthew J.
Derry
,
Andreas Haahr
Larsen
Diamond Proposal Number(s):
[39511]
Open Access
Abstract: Amphiphilic copolymers have emerged as powerful, detergent-free tools for solubilizing biological membranes, enabling the extraction and stabilization of membrane proteins within native-like lipid environments. We report a comprehensive, multi-technique elucidation of how polymer:lipid stoichiometry governs the formation, size, and stability of styrene-maleic acid lipid particles (SMALPs). Using commercial SMA2000, a styrene-maleic acid copolymer made using free radical polymerization and 1,2-ditetradecanoyl-sn-glycero-3-phosphocholine (DMPC) as a model phospholipid, we prepared SMALPs across a wide range of polymer-to-lipid weight ratios and employed an integrated suite of orthogonal characterization methods, including size exclusion chromatography (SEC), dynamic light scattering (DLS), flow-induced dispersion analysis (FIDA), mass photometry, ensemble and time-resolved Förster resonance energy transfer (FRET), and small-angle X-ray scattering (SAXS), to establish the structural consequences of varying polymer content. Our data reveal that efficient lipid solubilization into nanodiscs requires a minimum amount of polymer. Above ~1% (w/v) SMA2000: 1% DMPC, well-defined nanodiscs of ~10 nm diameter are formed that, on average, exhibit a consistent stoichiometry of ~130 lipids encircled by ~11 polymer chains. Through a new molecularly-constrained SAXS model, we show that these nanodiscs possess a stable bilayer height across variations in polymer to lipid ratio and a narrow polymer belt, and that their structural parameters remain invariant once excess polymer is used. In contrast, insufficient polymer (<1% w/v) generates bimodal populations including substantially larger discs. Notably, nanodiscs formed at optimal polymer:lipid ratios remain structurally stable for at least two months. Together, these results provide a rigorous quantification of SMALP composition and preferred size, enhancing our understanding of polymer-lipid nanodisc formation and offering critical design rules for detergent-free membrane protein extraction.
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Jul 2026
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E01-JEM ARM 200CF
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Emerson C.
Kohlrausch
,
Christopher
Leist
,
Gazi N.
Aliev
,
Mohsen
Danaie
,
Matthew
Young
,
Madasamy
Thangamuthu
,
Yifan
Chen
,
William J.
Cull
,
Wolfgang
Theis
,
Ute
Kaiser
,
Andrei N.
Khlobystov
,
Jesum
Alves Fernandes
Diamond Proposal Number(s):
[37379, 38763]
Abstract: Understanding how catalytically active sites emerge and evolve under working conditions is a fundamental challenge that limits the rational design of heterogeneous catalysts. Here, we directly visualize the transformation between alloyed PtNi and phase-separated Pt-NiO nanoclusters during hydrogen evolution. Using in situ low-voltage aberration-corrected electron microscopy, with the electron beam serving as both the stimulus and probe, we track the formation of active sites under low-water-vapor conditions. PtNi nanoclusters were assembled with controlled mixing of the atoms, resulting in two distinct configurational entropy states. Under reaction conditions, the transformation of bimetallic nanoclusters shifts from an entropically stabilized alloy to an enthalpically favored phase-separated configuration, controlled by oxygen availability and by a critical nucleus size. The atomic dynamics observed in real space correlate directly with catalytic performance, where the low-entropy Pt-NiO state achieves a record hydrogen evolution mass activity of 11.1 A/mgPt due to a high density of interfacial sites that promote water dissociation on NiO and efficient hydrogen adsorption on Pt atoms.
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Jun 2026
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I22-Small angle scattering & Diffraction
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Eleni
Axioti
,
Nana A.
Berfi
,
Philippa L.
Jacob
,
Klara M.
Saller
,
Georgia L.
Maitland
,
Anisha
Patel
,
Sri Nithya
Paruchuri
,
Paul D.
Topham
,
Matthew J.
Derry
,
Shreyasi
Chatterjee
,
Benoit
Couturaud
,
Luciano
Galantini
,
Iolanda
Francolini
,
Valentina
Cuzzucoli Crucitti
,
Veeren M.
Chauhan
,
Robert J.
Cavanagh
,
Vincenzo
Taresco
Diamond Proposal Number(s):
[38357]
Open Access
Abstract: Recent studies have highlighted the limitations of conventional high degrees of PEGylation in drug delivery systems, including immune recognition and reduced efficacy. Approaches such as poly(ethylene glycol) (PEG) isomerization and shortening of PEG chains have emerged as strategies to mitigate anti-PEG immune responses while preserving key physicochemical properties required for drug delivery. Inspired by these advancements, this study aims to enzymatically synthesize new hybrid polymers incorporating a limited fraction of PEG and biosourced polyols, such as glycerol and diglycerol, as the hydrophilic counterpart, minimizing the amount of PEG by 50% (compared to our previous work). These novel adipate-based tetrapolymers, generated using four different starting materials, outperformed previous systems, offering a tunable and sustainable design for nanomedicine. By strategically limiting the PEG fraction, we preserved the functional benefits of PEGylation, including stealth and amphiphilicity, while advancing toward greener chemistry. The resulting biodegradable PEGylated polyesters were formulated from film rehydration of solid dispersions and increased the water solubility of the model drug curcumin via direct encapsulation of the compound in polymeric nanoparticles. The best performing polymer variant consisted of diglycerol, 1,6-hexanediol, and PEG combined with divinyl adipate (PEGDGA-Hex 50%). Its drug interactions, colloidal stability, biodegradability, and biocompatibility, in both in vitro (Caco2, human intestinal epithelial cells MCF-7, human breast cancer cells, and MDA-MB-231 late-stage triple-negative breast cancer cells) and invertebrate in vivo models that align with 3R principles (Caenorhabditis elegans and Drosophila melanogaster), support its potential use in systemic drug delivery.
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Jun 2026
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B21-High Throughput SAXS
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Diamond Proposal Number(s):
[35502]
Open Access
Abstract: When nanoparticles (NPs) enter biological environments, they are rapidly coated by biomolecules, forming the protein corona (PC) that defines their biological identity and dictates how NPs are recognized, distributed, and processed by living systems. Capturing the authentic features of the PC demands experimental conditions that preserve its native state, which are difficult to achieve once NPs are removed from their biological milieu. Despite significant progress, current PC quantification methods still rely on separating the NP-PC complex from its native environment, thereby compromising the corona's integrity and preventing accurate evaluation of its physicochemical properties. Here, we introduce a fractionation-free approach based on synchrotron small-angle X-ray scattering (SAXS) to quantitatively determine the amount of protein adsorbed onto silica NPs under native conditions. By modeling the scattering contribution of free versus bound proteins, we directly extracted the adsorbed mass in both single-protein (serum albumin) and complex proteomic (human serum) systems. The resulting adsorption isotherms enabled the determination of thermodynamic parameters, distinguishing between simple monolayer-like and more complex adsorption regimes. Together, these findings establish SAXS as a non-invasive and quantitative technique for probing the PC in situ without perturbing equilibrium, advancing SAXS toward quantitative PC characterization.
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Jun 2026
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B18-Core EXAFS
E02-JEM ARM 300CF
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Donato
Decarolis
,
Sahra
Ahmed
,
James
King
,
Alin-Marin
Elena
,
Linda
Zhang
,
Jeff
Armstrong
,
Ines
Lezcano-Gonzalez
,
Mohsen
Danaie
,
Michael
Hirscher
,
Simone
Meloni
,
Andrew M.
Beale
,
Petra A.
Szilagyi
Diamond Proposal Number(s):
[42564]
Open Access
Abstract: Metal–organic frameworks have been intensively investigated for their ability to effectively control the growth and surface chemistry of nanosized guests, with their pores acting as templates and potentially providing anchoring sites. Since the speciation, as determined by the geometry and surface chemistry of hydride-forming metals, such as Pd, under particular conditions (T, p), is controlled by their size at and beyond the nanoscale, metal–organic frameworks are a prospective matrix for speciation or phase selection. This is of relevance because the role and characteristics of the phases in hydrogenation reactions involving hydride-forming Pd catalysts are open questions. In particular, it is a matter of debate which palladium phase is the most active and most selective, as they often occur simultaneously under catalytic conditions. For the first time, our thorough investigation, including operando XAFS and computer simulations, demonstrates that by embedding Pd nanoclusters, ≤1 nm in diameter, in the pores of the NH2–UiO-66 metal–organic framework, the speciation of subnanometric Pd particles can be controlled, such that the active particles only exist in their metallic state under reaction conditions; in fact, the Pd–H2 mixture only affords surface-bound hydrogen atoms. This control of Pd speciation consequently enables the direct probing of the phase activity and selectivity in the model reaction of 1,3-butadiene hydrogenation to butenes, wherein it showed no deactivation and improved selectivity compared to conventionally prepared catalytic systems. This result shows that the metallic phase can be stabilized through subnanometric size control and that it is more selective and less prone to overhydrogenating the butadiene reactant to butane, resulting in a purer product.
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Jun 2026
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I10-Beamline for Advanced Dichroism - scattering
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Open Access
Abstract: A series of exchange-coupled magnetic nanoparticles featuring multiple magnetic phases arranged in a core-shell architecture was synthesized through a three-step seed-mediated growth process. Iron, cobalt, and nickel precursors were sequentially thermally decomposed in high-boiling-point solvents (approximately 300 °C), enabling the successive growth of CoO and NiO shells on Fe₃−dO₄ nanoparticle's cores. The structural and chemical characteristics of these nanoparticles were thoroughly investigated using a combination of advanced analytical techniques, including scanning transmission electron microscopy in high-angle annular dark-field imaging mode (STEM-HAADF), electron energy-loss spectroscopy STEM (EELS-STEM), and X-ray magnetic circular dichroism (XMCD). After each thermal decomposition step, the nanoparticle size progressively increased, accompanied by noticeable changes in morphology, indicating significant surface reconstruction. Furthermore, the chemical structure proved to be more complex than initially anticipated. The high synthesis temperature promoted cation interdiffusion at the interfaces as well as partial dissolution–recrystallization processes at the nanoparticle surface. An intermixed Co/Ni shell, composed of a combination of wüstite and spinel phases, was found to strongly influence the magnetic properties of the nanoparticles through exchange bias coupling. This effect is directly correlated with the relative proportions of Co and Ni cations incorporated within the shell.
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Jun 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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I15-1-X-ray Pair Distribution Function (XPDF)
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Laura G.
Graversen
,
Nicolas
Schlegel
,
Freja B.
Holde
,
Adrian
Sanz Arjona
,
Stefanie
Punke
,
Tobias M.
Nielsen
,
Andy S.
Anker
,
Jonas
Forner
,
Gustav K. H.
Wiberg
,
Matthias
Arenz
,
Rebecca K.
Pittkowski
,
Kirsten M. Ø.
Jensen
Diamond Proposal Number(s):
[30653]
Open Access
Abstract: Iridium oxide nanoparticles are efficient catalysts for the acidic oxygen evolution reaction (OER). We present a straightforward one-pot hydrothermal synthesis method to produce sub-1 nm Ir oxide nanoparticles in a single step, with size control achieved through post-synthesis annealing. By combining X-ray total scattering and pair distribution function (PDF) analysis with small-angle X-ray scattering (SAXS), we find that the sub-nanometer-sized oxide has an increased number of edge-sharing [IrO6]-octahedra compared to the thermodynamically favorable rutile structure. PDF modelling using various cluster motifs reveals that a sheet-like cluster, derived from rutile and comprising seven [IrO6]-octahedra with a (110)-exposed surface, can describe the increased Ir–Ir edge-sharing connectivity. We further find that cluster growth leads to a decrease in the number of edge-sharing motifs, going towards the bulk rutile structure upon annealing. Operando X-ray total scattering and PDF analysis during OER reveal high structural stability of the ultra-small (<3 nm) Ir oxides.
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Jun 2026
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