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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E02-JEM ARM 300CF
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Diamond Proposal Number(s):
[31878, 33382, 34606, 34607]
Open Access
Abstract: Nanoscale phase separation in polymer semiconductor blends significantly influences their mechanical, optical, and transport properties, and uncontrolled phase separation ultimately contributes to the long-term degradation of devices. Recent advances in electron microscopy have enabled imaging and diffraction-based analysis of polymer components, but these approaches are typically limited to blends with components exhibiting sharp differences in crystallinity or molecular structure. Here, we employ low-dose scanning electron diffraction to characterize phase-separated domains of components with nearly identical molecular structure, namely poly(9,9-di-n-octylfluorenyl-2,7-diyl) (F8) and poly(9,9-dioctylfluorene-alt-benzothiadiazole) (F8BT). For semicrystalline blends, we demonstrate phase identification and crystallographic texture analysis. In fully amorphous systems with partial phase separation, we highlight the limitations of electron pair distribution function (ePDF) analysis. Instead, we exploit differences in angle-dependent scattering, coupled with calculated intramolecular scattering intensities, to reliably map distinct amorphous phases. Finally, we showcase this suite of techniques for characterizing a model device cross-section, prepared by cryogenic focused ion beam milling. These workflows decouple phase separation and crystallization processes in F8:F8BT blends, provide corroborating insights into F8 crystalline and amorphous intermolecular π − π stacking, and support the direct visualization of non-crystalline organic multilayer interfaces in cross-section needed for failure analysis in organic optoelectronics.
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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
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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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Aquilos-CryoFIB at Diamond
Scios-Scios at Diamond
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Diamond Proposal Number(s):
[35964]
Open Access
Abstract: Dragonfly- and cicada-wing-inspired titanium nanostructured surfaces exhibit promising bactericidal properties. However, direct visualization of the bacteria–material interface under hydrated conditions remains limited, restricting experimental interrogation of how bacteria interact with nanostructured surfaces. This limitation reflects a long-standing methodological gap, as visualization of bacteria–nanostructure interfaces has largely relied upon indirect or dehydrated imaging approaches. Cryo-electron tomography (cryo-ET) enables 3D visualization of cellular ultrastructure in a native hydrated environment, but imaging bacteria attached to metallic nanostructures by cryo-ET requires preparation of thin electron-transparent lamellae. Obtaining such lamellae from vitrified bacteria on titanium substrates is technically challenging because cryo-focused ion beam (cryo-FIB) milling must simultaneously section soft biological material and hard metal whilst bacteria embedded in vitreous ice are not directly visible. Here, we establish a correlative cryogenic workflow enabling targeted extraction and cryo-ET imaging of defined bacterium–nanopillar interfaces. Individual bacteria interacting with titanium nanopillars are identified by correlative cryo-fluorescence microscopy, followed by targeted cryo-FIB lift-out, transfer to a receiver grid, and thinning into electron-transparent lamellae. The data presented demonstrate that bacteria–nanostructure interfaces can be targeted, extracted, and structurally analysed in situ under fully hydrated conditions. This workflow provides a methodological framework for future cryo-ET studies of bacteria–nanotopography interactions.
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May 2026
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I10-Beamline for Advanced Dichroism - scattering
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Diamond Proposal Number(s):
[35696]
Open Access
Abstract: Magnetocrystalline anisotropy is a key parameter governing the performance of magnetic nanoparticles in many applications. However, disentangling its intrinsic contribution from other sources of effective anisotropy, such as surface effects, dipolar interactions or shape anisotropy, remains highly challenging. Here, we report a novel approach to qualitatively estimate the magnetocrystalline anisotropy of two CoxFe3−xO4 nanoparticles with different Co contents (x = 0.11 and 0.61) using polarized neutron powder diffraction (PNPD). The off-diagonal elements of the susceptibility tensors and degree of asymmetry of the magnetization ellipsoids obtained from the PNPD refinements reveal that the sample with x = 0.61 presents a larger magnetocrystalline anisotropy than the sample with x = 0.11, which is consistent with the effective anisotropy derived from magnetometry. Moreover, comparison of the PNPD-derived magnetization ellipsoids across materials with varying anisotropies confirms the direct relationship between the ellipsoid asymmetry and magnetocrystalline anisotropy. These findings establish PNPD as a powerful tool for qualitatively probing intrinsic anisotropies in nanoparticle systems, paving the way for the rational design and optimization of magnetic nanoparticles for advanced applications.
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May 2026
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B07-C-Versatile Soft X-ray beamline: Ambient Pressure XPS and NEXAFS
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Diamond Proposal Number(s):
[36218]
Open Access
Abstract: Controlling the redox landscape of transition metal oxides is central to advancing their reactivity for heterogeneous catalysis or high-performance gas sensing. Here, we report single Cu atom sites (1.42 wt.%) anchored on Co3O4 nanoparticles (Cu1-Co3O4) that dramatically enhance reactivity and molecular sensing properties of the support at low temperature. The Cu1 are identified by x-ray absorption near edge structure and feature metal–support interaction between the atomically dispersed Cu (mostly in 2+ oxidation state) and Co3O4, as revealed by x-ray photoelectron spectroscopy. The ability of Cu1 to form interfacial Cu–O–Co linkages strongly reduces the temperature of lattice oxygen activation compared to CuO nanoparticles on Co3O4 (CuONP-Co3O4), as demonstrated by temperature-programmed reduction and desorption analyses, in agreement with density functional theory calculations. To demonstrate practical impact, we deploy Cu1-Co3O4 nanoparticles as a chemoresistive sensor for formaldehyde that yields more than an order of magnitude higher response than CuONP-Co3O4 and consistently outperforms state-of-the-art sensors. Formaldehyde is detected down to 5 parts-per-billion at 50% relative humidity and 75°C with excellent selectivity over critical interferents. These results establish a strategy for activating redox-active supports using single-atom isolates of non-noble nature, yielding drastically enhanced and well-defined reactivity to promote low-temperature oxidation reactions and selective analyte sensing.
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Apr 2026
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I20-Scanning-X-ray spectroscopy (XAS/XES)
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Yuvraj
Vaishnav
,
Mohamad
Abou-Daher
,
Cristina I. Q.
Silva
,
Rohit K.
Rai
,
Walid
Al Maksoud
,
Marcell
Toth
,
Mohandoss
Viswanathan
,
Peng
Ren
,
Fumitaka
Takeiri
,
Shusaku
Hayama
,
Samy
Ould-Chikh
,
Mohamed Nejib
Hedhili
,
Maxim
Avdeev
,
Wen
Yin
,
Saburo
Hosokawa
,
Genki
Kobayashi
,
Isaac
Abrahams
,
Aamir
Farooq
,
Javier
Ruiz-Martinez
,
Yoji
Kobayashi
Diamond Proposal Number(s):
[31497]
Open Access
Abstract: High-entropy oxides are attracting attention for catalysis, but there are relatively few detailed studies on their precise structure, hampering true detailed studies on fundamental properties affecting their activities. In addition, diffusion has been often characterized as generally slow in high-entropy systems. Here, we determine the precise oxygen content and structure of the fluorite-like high-entropy oxide (La, Ce, Pr, Nd, Y)O1.68 and have identified a large oxygen storage capacity based on efficient Ce/Pr redox due to facile oxide diffusion pathways and suppression of sintering. The structure and composition were identified through a combined Rietveld refinement of X-ray and neutron diffraction data, and the oxidation state of Ce and Pr was investigated by high energy resolution fluorescence detected–X-ray absorption near edge spectra (HERFD–XANES). (La, Ce, Pr, Nd, Y)O1.68 utilizes the full redox range of Ce/Pr, resulting in a high oxygen storage cumulative capacity despite the lower content of Ce/Pr compared to other well-known ceria derivatives. Diffusion pathway analysis by bond valence site energy mapping shows decreased barriers for oxide anion diffusion through the bulk, also benefiting redox reactions. The high-entropy nature also suppresses sintering, resulting in better cycling performance. This results in a higher performance as a methane oxidation catalyst support. We also investigate its use as a NOx reduction catalyst support.
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Mar 2026
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E02-JEM ARM 300CF
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Diamond Proposal Number(s):
[37041, 56733]
Open Access
Abstract: 2D Prussian blue and its analogues hold great promise for applications in catalysis, energy conversion, sensing, and memory devices, thanks to their open frameworks, surface activity, and directional ion transport. However, synthesizing high-quality and large-area 2D films remains a major challenge. Here, we present a robust and scalable liquid-liquid interfacial synthesis that enables the formation of continuous, 2D flakes of Prussian blue (Fe3+[Fe2+(CN)6]0.75) with tunable thicknesses from ∼2 nm to several hundred nanometers. The controlled reduction of [Fe3+(CN)6]3− to [Fe2+(CN)6]4− enables slow, directed growth of 2D-FeFe layers. Unlike films formed from nanoparticles, this method yields high-quality flakes suitable for integration into devices. As a demonstration, we incorporated these films into Ag filament-based electrochemical metallization memristors. The 2D-FeFe devices ≥50 nm thick exhibited reliable bipolar electrical switching, with high Roff/on ratios (∼106), >6 h retention, and stability over 150 cycles. Strikingly, switching was observed across 1.5 µm lateral gaps, far exceeding conventional silver filament formation distances, highlighting the superior ion transport and structural integrity of these 2D frameworks. This scalable approach to 2D Prussian blue, which has the potential to be extended to other related coordination polymers, offers exciting opportunities beyond memristors, enabling integration into technologies where thin-film compatibility, directional ion transport, and high surface activity are critical, such as catalysis, energy storage, and neuromorphic computing.
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Jan 2026
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[33261]
Open Access
Abstract: Lithium metal (LM) and zero-excess lithium (ZE) anodes offer pathways to increase the energy density of all-solid-state batteries (ASSBs). We employ operando X-ray computed tomography combined with an image subtraction method to visualize lithium plating/stripping morphology, stack mechanical failure, and quantify the lithium reversibility in asymmetric Li6PS5Cl (LPSC)-based ASSBs. Lithium metal counter electrode (CE) and copper (Cu) working electrode (WE) emulate LM and ZE interface configurations, respectively. We compare bare Cu and silver-coated Cu (Ag/Cu) WEs under varying current densities. At 0.25 mA cm−2(WE), bare Cu shows edge-localized and non-uniform lithium deposition, while Ag/Cu facilitates more uniform lithium spreading, but results in higher first-cycle irreversibility and lower Coulombic efficiency. Above 0.5 mA cm−2(WE), failure in Li|LPSC|Cu cells initiate at the LPSC|Cu interface via spallation cracks. In contrast, Ag preserves interface integrity at the WE despite lithium initially plates at discrete nucleation spots. However, failure shifts to the Li|LPSC interface, where non-uniform lithium depletion at the CE exposes the underlying Cu, leading to spallation cracks upon subsequent plating. Mechanical finite element simulations support these observations and underscore the critical role of the nucleation layers in mitigating mechanical failure. This study highlights interface engineering as a key strategy to address electro-chemo-mechanical degradation in LM- and ZE-ASSBs.
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Jan 2026
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B21-High Throughput SAXS
I22-Small angle scattering & Diffraction
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Abdulwahhab
Khedr
,
Mohamed A. N.
Soliman
,
Alfred
Corrigan
,
Tarsem
Sahota
,
Rachel
Armitage
,
Natalie
Allcock
,
Jeyapriya T.
Jegadeesan
,
Mahetab H.
Amer
,
Reem
Alazragi
,
Zeeshan
Ahmad
,
Jacek K.
Wychowaniec
,
Mohamed A.
Elsawy
Diamond Proposal Number(s):
[28287, 28806]
Open Access
Abstract: Multicomponent peptide nanostructures offer a powerful platform for designing functional materials, yet controlling their co-assembly remains a key challenge. Here, we harness electrostatic molecular recognition to drive the selective co-assembly of five amphiphilic ionic peptide binary mixtures (M1–M5). Our results revealed that charge distribution governs β-sheet strand alignment (parallel vs. antiparallel), assembly kinetics, and hydrogel viscoelasticity. Mixing stoichiometry and pH significantly influences co-assembly behavior, nanofiber morphology, and network structure (self-sorted vs. hetero-aggregated). At pH 7, equimolar mixtures undergo nucleation-driven co-assembly into hetero-aggregates, immediately forming well-defined nanofibers, while non-equimolar ratios yield altered morphologies. At a slightly acidic pH of 5–7, both E and K side chains are charged, enabling complementary ionic interactions that promote co-assembly and gelation. Outside this pH range, co-assembly is impaired. Notably, M1 forms β-sheets and hydrogels at acidic pH (≤4) via independent self-assembly of its components, suggesting self-sorted fibers. Overall, we demonstrate that tuning charge complementarity, ionization state, and stoichiometry enables precise control over the molecular, nanoscale, and mechanical properties of multicomponent peptide assemblies, providing a framework for the rational design of advanced peptide-based materials.
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Jan 2026
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