B07-B1-Versatile Soft X-ray beamline: High Throughput ES1
|
Diamond Proposal Number(s):
[43895]
Open Access
Abstract: X-ray photoelectron spectroscopy (XPS) is a major technique in catalyst research due to its ability to determine chemical states on the surface. Near ambient pressure XPS (NAP-XPS) enables in situ analysis, offering valuable insight into catalytic processes. However, modern catalysts are often supported on non-conductive supports such as TiO2 or SiO2, which can present significant challenges for XPS analysis due to charging and differential charging. These issues can distort spectral data, rendering data unusable and wasting valuable instrument time. While several sample preparation strategies exist, many are limited by not allowing high temperature analysis, the risk of sample loss (e.g., from powder flaking off), or continued susceptibility to charging. In this work, we introduce a simple, robust, and time-efficient method for mounting catalyst powders by compressing them between aluminium foil disks. This approach provides excellent sample hold, minimises charging effects, and is suitable for high-temperature NAP-XPS analysis and synchrotron x-ray sources. The method addresses key limitations of conventional preparation techniques and enables more reliable characterisation of insulating catalyst materials.
|
Aug 2026
|
|
B16-Test Beamline
|
Diamond Proposal Number(s):
[36299, 34545]
Open Access
Abstract: This study investigates the lattice strain induced by Ge:Sb alloy films on Ge substrates. Metastable films are formed by UV pulsed laser melting (PLM) of a Sb-coated Ge substrate. We fabricate thin Ge:Sb layers, systematically varying processing parameters and crystal orientation to study strain and strain-relaxation-induced defects. High-resolution X-Ray diffraction and electrical characterization revealed extremely high strain values as well as ultra-low resistivity induced by Sb. Maximum strain before the onset of strain relaxation was found to depend on crystal orientation with the Ge (1 1 1) orientation yielding the highest strain values. By combining structural as well as electrical information, we estimated Sb contribution to lattice expansion, separating electronically active from inactive fractions. Strain optimization was applied to an innovative application that is the production of bent crystals for high energy particle beam deflection and radiation production. Bending tests on thin Ge substrates confirmed the method, with controlled PLM processing allowing inducing quantifiable curvature with smallest achievable radii of 4.5 m. Exploiting non-equilibrium doping/alloying to exceed equilibrium Sb solubility is promising for applications ranging from ultra-low-resistivity layers in scaled nano-electronic devices to bent crystals for advanced systems like crystal-based undulators, enabling new approaches to high-energy photon production.
|
Jun 2026
|
|
I03-Macromolecular Crystallography
|
Olesia
Werbowy
,
Maria
Håkansson
,
Sebastian
Dorawa
,
Aleksandra
Stefańska-Kaźmierczak
,
L. Anders
Svensson
,
Salam
Al-Karadaghi
,
Agata
Jurczak-Kurek
,
Karolina
Kwiatkowska-Semrau
,
Magdalena
Plotka
,
Olafur H.
Fridjonsson
,
Gudmundur O.
Hreggvidsson
,
Arnthór
Aevarsson
,
Sławomir
Dąbrowski
,
Anna‐karina
Kaczorowska
,
Tadeusz
Kaczorowski
Diamond Proposal Number(s):
[23282]
Abstract: We present the structural and functional characterization of a single-stranded DNA-binding protein (SSB-M5) identified from a hot spring metagenome in Vatnajökull National Park, Iceland. This small protein (136 aa; 15,695 Da) shares 100% amino acid sequence identity with two previously uncharacterized SSBs from hyperthermophilic Fervidobacterium species. Functional complementation assay demonstrated that SSB-M5 can substitute for Escherichia coli SSB in an ssb− mutant strain, confirming its biological activity. A recombinant C-terminally His-tagged SSB-M5 was overproduced, purified to homogeneity, and subjected to structural, biochemical, and biophysical analysis. The crystal structure revealed that SSB-M5 forms a dimer through a crystallographic twofold axis, with each monomer contributing to a large antiparallel β-sheet. The flat surfaces of the β-sheets from the two dimers are packed together via a second crystallographic twofold axis, forming a tetramer that serves as the functional unit of the SSB-M5. Electrophoretic mobility shift assays showed that SSB-M5, after heat treatment up to 100°C, forms stable DNA-protein complexes with the (dT)40 oligo. Quantitative analyses revealed that SSB-M5 binds (dT)70 oligonucleotide with very high affinity (KD = 72 ± 6 pM). Hill analysis indicated cooperative binding, yielding an EC50 of 141 pM and a Hill coefficient of 2. Moreover, inclusion of SSB-M5 in PCR reactions significantly enhanced amplification by eliminating non-specific products. Together, these findings identify SSB-M5 as a hyperthermostable, high-affinity single-stranded DNA-binding protein with potential applications in molecular biology and biotechnology.
|
Apr 2026
|
|
B21-High Throughput SAXS
|
Diamond Proposal Number(s):
[36130]
Open Access
Abstract: Shwachman-Diamond syndrome (SDS) is a rare genetic disorder characterized by pancreatic insufficiency and neutropenia. While most cases are linked to mutations in the SBDS gene, some involve mutations in the GTPase EFL1. This protein works with SBDS to release the anti-association factor eIF6 from the 60S ribosomal subunit during ribosome biogenesis. The pathogenic EFL1 R1095Q mutant (R1086Q in yeast) exhibits altered guanine nucleotide recognition and impaired eIF6 release, prompting an investigation into its structural consequences. Using the yeast Efl1 orthologue in X-ray hydroxyl radical footprinting experiments, we tracked changes in solvent accessibility caused by the mutation. Although the mutation is situated in domain IV, widespread conformational changes were observed across the protein, particularly in domain I, suggesting a long-range intramolecular communication. Strikingly, the growth defect caused by the pathogenic mutation was rescued by a second mutation located in a allosteric pathway that spans from the nucleotide-binding pocket to domain IV. This compensatory mutation restored proper nuclear localization of eIF6 (Tif6 in yeast). These findings reveal that the R1086Q mutation disrupts a structural communication network within Efl1, impairing the conformational dynamics required for its activity. The loss of this coordination likely underlies the ribosome maturation defects observed in SDS cases linked to EFL1, offering new insights into the molecular basis of the disease.
|
Apr 2026
|
|
I16-Materials and Magnetism
|
Diamond Proposal Number(s):
[24570]
Open Access
Abstract: Although there have been several studies on the powder form, there has yet to be a report on the bulk crystal growth and its property studies of LiNiO2. In the present study, we report the first successful growth of a LiNiO2 single crystal by employing the optical floating-zone technique. Structural properties have been studied using single-crystal X-ray diffraction (XRD). The structural refinement of the single-crystal XRD data, along with the Laue diffraction patterns, confirms that this system crystallizes in a rhombohedral unit cell in space group R3m and the presence of a single grain along the length of the grown crystal. Furthermore, for the first time, we have observed and determined their superstructures as a function of temperature using single-crystal XRD. We have also conducted a study using the high flux of synchrotron X-rays to demonstrate the mechanism which drives the superstructure witnessed by the single-crystal XRD. Resonant elastic X-ray scattering was used to confirm the superstructure and the mixed valence state of different Ni sites. No additional ordering phenomena were observed, including magnetic or electronic ordering. Our study demonstrates the optimization of LiNiO2 growth parameters and provides information about atomic and electronic ordering in the system, including the onset of a superstructure phase. This will provide a basis for further work in developing improved cathode materials and understanding quantum spin liquids.
|
Apr 2026
|
|
E02-JEM ARM 300CF
|
Sam
Sullivan-Allsop
,
Nick
Clark
,
Wendong
Wang
,
Rongsheng
Cai
,
William
Thornley
,
David G.
Hopkinson
,
James G.
Mchugh
,
Ben
Davies
,
Samuel
Pattisson
,
Nicholas F.
Dummer
,
Rui
Zhang
,
Matthew
Lindley
,
Gareth
Tainton
,
Jack
Harrison
,
Hugo
De Latour
,
Joseph
Parker
,
Joshua
Swindell
,
Eli G.
Castanon
,
Amy
Carl
,
David J.
Lewis
,
Natalia
Martsinovich
,
Christopher S.
Allen
,
Mohsen
Danaie
,
Andrew J.
Logsdail
,
Vladimir
Fal’ko
,
Graham J.
Hutchings
,
Alex
Summerfield
,
Roman
Gorbachev
,
Sarah J.
Haigh
Diamond Proposal Number(s):
[33252, 35552]
Abstract: The structure and dynamics of adsorbed atoms (adatoms) at solid-liquid interfaces determine the performance of advanced catalysts, electrochemical devices, molecular separation technologies, and metal extraction from waste streams. However, in situ investigations of atomically dispersed metals in various chemical environments have been prevented by insufficient imaging resolution and solvent incompatibility. In this study, we combined a specimen design that provides atomic resolution in liquid-phase electron microscopy with deep learning–enabled analysis to explore the interactions between gold adatoms, graphite support, and the solvent collectively. We tracked the locations of >106 graphite-supported gold adatoms, dimers, and larger clusters in five solvents. Although their initial atomic dispersion was determined by the solvent polarity, fast drying kinetics at low temperature was required for optimizing catalytic performance.
|
Apr 2026
|
|
Metrology
Optics
|
Open Access
Abstract: Advanced metrology methods are continually being developed and refined to meet the demanding quality standards of high-performance X-ray mirrors. Among these, interferometric techniques are the most widely used for measuring the height maps of optical surfaces. However, they often encounter limitations when applied to strongly curved or freeform surfaces, primarily due to high fringe density caused by steep slope. To address these challenges, we have developed a laser Speckle-based Curvature Optical Metrology instrument (SCOM) for measuring the two-dimensional surface curvature maps. This technique offers an alternative for characterizing complex optical surfaces by using a digital image correlation algorithm to extract curvature information from the speckle pattern, which effectively acts as a set of wavefront markers. We have demonstrated the effectiveness of this method for measuring strongly curved mirrors with a radius of curvature from 10 m down to 100 mm. Additionally, we have applied this technique to online deterministic figuring of optical surfaces, in-situ stress measurements during multilayer deposition processes, and the characterization of deformable mirrors. This technique shows great promise not only for high precision metrology of X-ray mirrors used in synchrotron radiation facilities, free-electron lasers, and space and astronomical observatories, but also for freeform optical components in advanced industrial applications.
|
Apr 2026
|
|
I18-Microfocus Spectroscopy
|
Diamond Proposal Number(s):
[36744]
Open Access
Abstract: The integration of nanoencapsulation techniques with foliar application presents a promising approach to enhance selenium (Se) biofortification in agriculture. This study examined the foliar uptake of liposome-encapsulated Se in wheat leaves (Triticum aestivum) using synchrotron-based micro-X-ray fluorescence (μ-XRF) and confocal microscopy. μ-XRF mapping showed Se accumulation at leaf edges after 24 h, suggesting initial uptake via stomata, while free Se was absorbed and transported more rapidly, highlighting the slow-release effect provided by liposomal encapsulation, longer than the analyzed time. No immediate translocation of Se to the stem was observed, suggesting that more time is required for this internal movement. Micro-X-ray absorption near-edge structure (μ-XANES) speciation analysis demonstrated that Se was metabolized into organic forms within the plant. Finally, confocal fluorescence microscopy confirmed liposome absorption through the plant surface within 24 h, corroborating the μ-XRF findings. These results are crucial for optimizing liposome formulation to maximize Se transfer to edible parts.
|
Mar 2026
|
|
I09-Surface and Interface Structural Analysis
|
Muhammad
Ans
,
Eleni
Fiamegkou
,
Ashok S.
Menon
,
Gaurav C.
Pandey
,
Gaolo J.
Paez Fajardo
,
Harry
Gillions
,
Paolo
Melgari
,
Calum
Clenahan
,
Satish
Bolloju
,
Pardeep K.
Thakur
,
Tien-Lin
Lee
,
Serena A.
Cussen
,
Beth I. J.
Johnston
,
Louis F. J.
Piper
Diamond Proposal Number(s):
[38340]
Open Access
Abstract: Lithium nickel oxide (LNO) cathodes offer high capacity for high-energy-density applications but suffer rapid degradation above 4.2 V due to surface and bulk instabilities. Here, we apply an ultrathin aluminum oxide coating using powder atomic layer deposition to improve surface stability. Pouch cell testing shows that coated LNO delivers improved cycling behavior, retaining 91.2% capacity after 100 cycles at C/3. Operando X-ray diffraction reveals that after aging, coated LNO undergoes a less kinetically hindered delithiation, indicating that the surface coating further provides a surface-to-bulk stabilization effect. Postmortem surface sensitive spectroscopy confirms that the aluminum oxide layer (1) scavenges hydrofluoric acid and (2) suppresses surface reconstruction, reducing impedance growth and improving the surface integrity. Overall, the results demonstrate that ultrathin aluminum oxide coatings effectively mitigate interfacial degradation and enhance bulk electrochemical kinetics, providing an effective and scalable approach toward improving the long-term performance of ultra-Ni-rich cathodes.
|
Mar 2026
|
|
B21-High Throughput SAXS
|
Diamond Proposal Number(s):
[29895]
Open Access
Abstract: A lipopeptide is designed that contains an epitope from simian virus T-antigen (SV40T, PKKKRKV) conjugated to an N-terminal palmitoyl (C16-) moiety, with the aim to act as an effective cell-penetrating lipopeptide, with additional aggregation propensity conferred by the lipid chain. A combination of cryo-TEM and small-angle X-ray scattering (SAXS) is used to show that the lipopeptide forms micelles, but mixtures with DNA lead to formation of fractal cluster-like co-assemblies due to intercalation of the DNA and peptide. Spectroscopic studies using fluorescence and circular dichroism (along with fiber X-ray diffraction) show that the peptide interacts with DNA and inserts into the groove. Confocal microscopy along with flow cytometry confirms delivery of DNA into both HeLa and mouse embryonic stem cells (mESCs) in pluripotent state, and the system shows excellent cytocompatibility as confirmed by MTT assays. Our data indicate that the lipopeptide may outperform the DNA transfection agent lipofectamine in DNA delivery into these stem cells and it enables DNA delivery into the cytoplasm and nucleus.
|
Mar 2026
|
|
