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]
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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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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I07-Surface & interface diffraction
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Olivia
Gough
,
Katherine
Trinkaus
,
Pascal
Kaienburg
,
Zhenlong
Li
,
Andrea E.
Lauritzen
,
Jonathan
Rawle
,
Hugo
Norris
,
James
Hilfiker
,
Joel
Smith
,
Alessandro
Veneri
,
Gregory
Su
,
Moritz
Riede
Diamond Proposal Number(s):
[30773, 32922]
Abstract: The microstructure of organic small molecule (SM) layers in organic solar cells (OSCs) strongly influences device performance by impacting light absorption, charge transport, and recombination. We demonstrate that ellagic acid (EA), a naturally derived templating layer, induces substantial morphological and thus optoelectronic changes in the vacuum thermally evaporated (VTE) donor molecule DCV5T-Me(3,3). Using in situ grazing incidence wide-angle X-ray scattering (GIWAXS) during thin film deposition in the purpose-built MINERVA VTE chamber at Diamond Light Source, we show that a 5 nm EA layer reorients DCV5T-Me from an edge-on to a face-on molecular packing motif. This templating effect persists for up to around 90 nm of film thickness.
Through UV-vis spectrophotometry and photoluminescence (PL) spectroscopy, we observe a shift towards H-aggregation and decreased light absorption in the donor molecule with the EA template. Atomic force microscopy (AFM) shows that the donor morphology changes as a function of thickness from the donor-templating interface. In DCV5T-Me(3,3):C60 bulk heterojunction devices, the EA layer helps retain donor crystallinity and enhances short circuit current (J
), despite the lower absorption. Maximum power conversion efficiency in our devices is achieved with a 5 nm templating layer, which provides sufficient structural templating while maintaining partial interfacial contact for efficient charge extraction. We hypothesise that the improvement in J
is likely driven by enhanced charge carrier dynamics due to the orientation change, shift toward H-aggregation, and change in growth mode.
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Jun 2026
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labSAXS-Offline SAXS and Sample Environment Development
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Diamond Proposal Number(s):
[34017, 37151, 39136]
Open Access
Abstract: Alpha olefin sulfonate (AOS) is a widely used anionic surfactant, yet its phase behaviour has not previously been systematically mapped. Here, a comprehensive phase diagram is constructed over a concentration range of 2–70 wt% and temperatures from 25 to 80 °C using cross-polarized optical microscopy and small-angle X-ray scattering (SAXS). Polarized microscopy was used to delineate isotropic and anisotropic regions and identify phase boundaries, while SAXS provided quantitative structural characterisation, including lattice parameters, electron density reconstructions, and micellar size and shape analysis. Measurements were performed in sealed capillaries under controlled thermal conditions, with refined temperature increments used to resolve phase transitions. Five distinct phases were identified with decreasing water content: a micellar dispersion; a 2D hexagonal phase; a 2D ribbon phase; a previously unreported 3D hexagonal phase; and two lamellar phases. This temperature- and concentration-dependent sequence is structurally analogous to that of sodium dodecyl sulfate (SDS), though key distinctions arise from the molecular architecture of AOS, which promotes unique intermediate mesophases through differences in molecular packing and constrained hydration. Structural analysis reveals a systematic evolution of spatial water organisation, progressing from excess bulk water in the micellar phase, to tubular confinement within hexagonal and ribbon phases, to discrete water pockets embedded within surfactant bilayers in the 3D hexagonal phase, and finally to residual interfacial hydration in the lamellar phases. This work establishes the relationship between hydration state and mesophase structure, and provides the first complete structural phase diagram for this important surfactant system, enabling prediction of phase behaviour under the complex conditions encountered in industrial processing.
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Jun 2026
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I21-Resonant Inelastic X-ray Scattering (RIXS)
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Kunhao
Li
,
Qizhi
Li
,
Changwei
Zou
,
Jaewon
Choi
,
Chaohui
Yin
,
Mirian
Garcia-Fernandez
,
Stefano
Agrestini
,
Shilong
Zhang
,
Chengtian
Lin
,
Xingjiang
Zhou
,
Ke-Jin
Zhou
,
Yi
Lu
,
Yingying
Peng
Diamond Proposal Number(s):
[30361]
Abstract: The superconducting gap is a characteristic feature of high-𝑇c superconductors and provides crucial information on the pairing mechanism underlying high-temperature superconductivity. Here, we employ high-resolution resonant inelastic x-ray scattering (RIXS) at the Cu 𝐿3 edge to investigate the superconducting gap in the overdoped cuprate Bi2Sr2Ca2Cu3O10+𝛿 (𝑇c=107K). By analyzing antisymmetrized, temperature-dependent RIXS spectra over a range of in-plane momentum transfers, we observe a clear suppression of low-energy spectral weight below 𝑇c, indicative of superconducting-gap formation. This suppression is most pronounced at small momentum transfers [
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𝒒∥
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≤0.18 r.l.u. (reciprocal lattice units)] and corresponds to a gap size of approximately 2Δ0∼130 meV. Comparison with theoretical calculations of the momentum-dependent charge susceptibility supports a 𝑑-wave symmetry of the superconducting gap, while an isotropic 𝑠-wave gap fails to reproduce key experimental features. These findings establish RIXS as a powerful, bulk-sensitive probe of superconducting-gap symmetry and highlight its utility for studying materials beyond the reach of surface-sensitive techniques such as ARPES and STM.
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Jun 2026
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I15-1-X-ray Pair Distribution Function (XPDF)
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Clara
Chinchilla-Garzó
,
Eva
Rivera-Chao
,
Miguel
Gomez-Mendoza
,
Bruno J. C.
Vieira
,
Neyvis
Almora-Barrios
,
Pol
Gimeno-Fonquernie
,
Javier
Castells-Gil
,
Rebecca
Vismara
,
Jan
Navrátil
,
Piotr
Błoński
,
Víctor A.
De La Pena O'Shea
,
João C.
Waerenborgh
,
Carlos
Marti-Gastaldo
,
Natalia
M. Padial
Diamond Proposal Number(s):
[40138]
Abstract: Photoredox catalysis has emerged as a powerful strategy for promoting redox reactions under mild conditions, but its translation from homogeneous to heterogeneous catalysts in porous solids remains limited. Metal-organic frameworks (MOFs) offer unique opportunities to bridge this gap by combining tailorable photoactive architectures with high stability, large surface areas, and modular control over reactivity via component selection. Despite recent progress, most photocatalytic MOF-based systems have focused on water splitting or CO2 reduction, whereas applications in organic synthesis remain virtually unexplored. Here, we report a titanium-iron MOF (MUV-1001) built from heterometallic TiFe2 metal-oxo clusters that operates as an intrinsically active visible-light photoredox catalyst. This platform enables single-electron transfer reactivity under irradiation, as demonstrated in a decarboxylative Giese reaction, and it represents an example of noble-metal- and additive-free C–C bond formation mediated by a pristine crystalline reticular material. Our findings highlight the potential of cluster-based design to access intrinsically photoactive systems, where subtle changes in composition dictate reactivity, even across isostructural families.
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Jun 2026
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I07-Surface & interface diffraction
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Diamond Proposal Number(s):
[39429]
Abstract: Formamidinium lead iodide (FAPbI3), which has a narrower band gap close to the Shockley-Queisser limit, offers higher power conversion efficiency (PCE) than other perovskite compositions, surpassing 27% [1]–[3]. However, under external stressors like moisture in ambient air processing conditions, its high tolerance factor value causes phase instability because of the larger ion size of FA+ [4]–[6]. Additionally, a higher annealing temperature (>390 K) is needed to reach the cubic α-phase of FAPbI3, whereas lower temperatures result in the formation of a non-photoactive δ-phase [7].
In recent years, FAPbI3 perovskite ink has been extensively incorporated with volatile methylammonium chloride (MACl) as a transitional stabilizer [8]. This substance effectively provides FAPbI3 black phase without annealing by decreasing the formation energy. However, the advantageous effects of MACl as an α-phase FAPbI3 inducer and stabilizer at room temperature are neutralized under ambient conditions and in the presence of non-volatile coordinating DMSO, which is frequently used as a co-solvent with toxic DMF to regulate the crystallization process [9]. DMSO accelerates the α-to-δ phase transition in air by displacing MACl from the intermediate film through the formation of stronger bonds with PbI2.
In this work, we use recently emerged Triethyl Phosphate (TEP) as a green solvent to dissolve FAPbI3 precursors and in-situ study its crystallization kinetics in the presence of MACl and excess PbI2 under ambient condition using transmission wide angle x-ray scattering (T-WAXS) [10] and steady-state photoluminescence (PL) techniques. Our results show that, unlike DMSO containing solvent systems, TEP with appropriate coordination ability allows for direct solvent extraction during anti-solvent quenching process avoiding intermediate phase formation. Furthermore, it has been found that the addition of excess PbI2 to the perovskite solution, along with MACl, not only regulates the pre-nucleation stage, leading to larger and more ordered crystals, as opposed to MACl alone as an additive, but also accelerates the formation of α-phase FAPbI3 at room temperature and stabilizes it under ambient condition during spin casting. This study paves the way for achieving high efficiency FAPbI3 solar cells using a non-toxic solvent system and under ambient conditions.
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May 2026
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I21-Resonant Inelastic X-ray Scattering (RIXS)
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Gaurav C.
Pandey
,
Ashok S.
Menon
,
Valeria
Calani San Miguel
,
José J.
Arroyo‐gómez
,
Harry
Gillions
,
Rebecca
Sellers
,
Matthew J. W.
Ogley
,
Eleni
Fiamegkou
,
Satish
Bolloju
,
Sahil
Tippireddy
,
Mirian
Garcia-Fernandez
,
Steven
Huband
,
Louis F. J.
Piper
Diamond Proposal Number(s):
[38432]
Open Access
Abstract: The electrochemical performance of single-crystalline (SC) Ni-rich layered oxide cathodes is fundamentally limited by bulk Li+ diffusion within micrometre-sized particles. During high-voltage cycling—necessary for high-energy applications—intraparticle Li+ diffusion is further impeded by oxygen-loss-induced surface reconstruction from the layered phase to spinel/rock-salt structures. Therefore, to fully understand how bulk Li+ transport kinetics influences electrochemical degradation, it is necessary to establish the correlation between surface reconstruction and bulk delithiation during the anisotropic structural evolution (i.e., expansion of the layers followed by their contraction) of the cathode particles during long-term cycling. In this work, we accomplish this using multi-rate operando X-ray diffraction studies of SC Ni-rich layered oxide cathodes aged under different voltage windows in single-layer pouch full cells. We quantify how increased surface reconstruction leads to greater heterogeneity in bulk delithiation, thereby promoting phase separation and exacerbating electrochemical capacity fade. These results provide a direct mechanistic link between surface degradation and bulk delithiation in such cathodes and offer a framework for non-destructively probing kinetics-dependent degradation under practically relevant conditions to guide strategies for improved cycling stability.
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May 2026
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I22-Small angle scattering & Diffraction
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Diamond Proposal Number(s):
[34844, 37870]
Open Access
Abstract: Fats are essential ingredients widely used in the food industry, as well as in cosmetic and pharmaceutical formulations. Solid fats are complex multicomponent systems primarily composed of triacylglycerols (TAGs), which determine the types and properties of the crystalline structures formed. TAGs crystallize in different polymorphs and stacking configurations, with distinct thermal and mechanical properties that influence the macroscopic structure and sensory profile of fat-based products. In this study, a comprehensive multi-technique analysis of animal-derived fats, specifically chicken and beef fats, was conducted. Chemical characterization was performed and solid fat content (SFC) was determined. Thermal behaviour was investigated using differential scanning calorimetry (DSC), whereas crystallization experiments were conducted using in situ turbidity measurements and synchrotron small-angle and wide-angle x-ray scattering (SAXS/WAXS) for structural characterization. Three different synchrotron experimental setups were used for crystallization experiments, including static and sheared conditions. The results demonstrate that the crystallization behaviour of beef and chicken fat samples closely correlate with their TAGs composition. Synchrotron x-ray scattering provided structural insights, highlighting how the polymorphic behaviour is influenced by fat origin and crystallization conditions. For both animal fat types, all three main polymorphs and possible transitions were detected. Moreover, the presence of shear promoted crystallization of stable polymorphs.
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May 2026
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I21-Resonant Inelastic X-ray Scattering (RIXS)
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Diamond Proposal Number(s):
[29150]
Open Access
Abstract: Cuprate superconductors show various collective charge correlations that are intimately connected with their electronic properties. In particular, charge order in the form of an incommensurate charge density wave (CDW) order with an in-plane wave vector 𝛿CDW≈0.23–0.35 reciprocal lattice units appears to be universally present. In addition to CDW, dynamic charge density fluctuations (CDFs) are also present with wave vectors comparable to 𝛿CDW. CDFs are present up to ≈300K and have relatively short correlation lengths of 𝜉≈20Å. Here we use Cu-𝐿3 and O-𝐾 resonant inelastic x-ray scattering (RIXS) to study the doping dependence of CDW and CDFs in La2−𝑥Sr𝑥CuO4. We fit our data with (quasi)elastic peaks resulting from the CDW and up to four inelastic modes associated with oxygen phonons that can be strongly coupled to the CDFs. Our analysis allows us to separate the charge correlations into three components: the CDW with wave vector 𝛿4𝑎-CDW≈0.24 and two CDF components with 𝛿4𝑎-CDF≈0.24 and 𝛿3𝑎-CDF≈0.30. We find that for 𝑇≈𝑇𝑐 the CDW coexists with the CDFs for dopings near 𝑥=𝑝≈1/8. The 4𝑎-CDW disappears beyond 𝑥=0.16 and the 4𝑎-CDF beyond 𝑥=0.19, leaving only a weak 3𝑎-CDF at the highest doping studied, 𝑥=0.22. Our data suggest that low-energy charge fluctuations exist up to doping 𝑥=0.19=𝑝★, where the pseudogap disappears; however, we find no evidence that they are associated with a quantum critical point.
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May 2026
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