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91 items found (0 items not approved), displaying 1 to 10.[First/Prev] 1, 2, 3, 4, 5, 6, 7, 8 [Next/Last]

Instruments / Technical Area	Publication Details	Published
I14-Hard X-ray Nanoprobe	Visualization of soil aggregate structures provides insights into their formation mechanisms induced by litter inputs Milda Pucetaite , Per Persson , Julia Parker , Ulf Johansson , Edith C. Hammer Soil Biology And Biochemistry 187 DOI: 10.1016/j.soilbio.2024.109686 Diamond Proposal Number(s): [27292] Open Access Show Abstract ▼ Abstract: Soil aggregation is a dynamic process influenced by physical, chemical and biological factors; however, their individual and combined effect on the formation and turnover of aggregates is not well understood. The aim of this study was to examine incorporation of fresh litter inputs of different physicochemical properties including their carbon-to-nitrogen (C/N) ratio – maize (C/N = 12) and straw (C/N = 103) - into aggregates, de novo formed from mineral soil with or without the presence of microbiota. Using rare-earth element oxides, we labelled structures formed during a four-week incubation with a single litter type and traced their incorporation into newly formed aggregates after mixing them together and incubating for a subsequent seven-week period. To visualize them, we used synchrotron-based X-ray fluorescence microspectroscopy, which allowed us to demonstrate that presence of the plant-derived particulate organic matter was the key factor for the aggregate formation. Within the timescale of the experiment, neither microbial abundance nor the community composition had any significant effect. However, the relative increase in straw-associated soil in aggregates larger than 250 μm provided support for our hypothesis regarding impact of carbon-rich organic matter on macroaggregation, likely via promotion of fungal growth and hyphal enmeshing. Phospholipid fatty acid analysis further confirmed relatively higher abundance of fungi in macroaggregates in straw-containing soil. All in all, our study provides insights into the initial stages of aggregate formation following litter additions and development of associated microbial community. The spatial analysis enabled by the X-ray fluorescence microspectroscopy enabled visualization of internal aggregate structures, shedding light on the processes involved, which is not possible with bulk analysis alone.	Dec 2024
I14-Hard X-ray Nanoprobe	The impact of interfacial quality and nanoscale performance disorder on the stability of alloyed perovskite solar cells Kyle Frohna , Cullen Chosy , Amran Al-Ashouri , Florian Scheler , Yu-Hsien Chiang , Milos Dubajic , Julia E. Parker , Jessica M. Walker , Lea Zimmermann , Thomas A. Selby , Yang Lu , Bart Roose , Steve Albrecht , Miguel Anaya , Samuel D. Stranks Nature Energy 580 DOI: 10.1038/s41560-024-01660-1 Diamond Proposal Number(s): [30427, 31964] Open Access Show Abstract ▼ Abstract: Microscopy provides a proxy for assessing the operation of perovskite solar cells, yet most works in the literature have focused on bare perovskite thin films, missing charge transport and recombination losses present in full devices. Here we demonstrate a multimodal operando microscopy toolkit to measure and spatially correlate nanoscale charge transport losses, recombination losses and chemical composition. By applying this toolkit to the same scan areas of state-of-the-art, alloyed perovskite cells before and after extended operation, we show that devices with the highest macroscopic performance have the lowest initial performance spatial heterogeneity—a crucial link that is missed in conventional microscopy. We show that engineering stable interfaces is critical to achieving robust devices. Once the interfaces are stabilized, we show that compositional engineering to homogenize charge extraction and to minimize variations in local power conversion efficiency is critical to improve performance and stability. We find that in our device space, perovskites can tolerate spatial disorder in chemistry, but not charge extraction.	Oct 2024
I14-Hard X-ray Nanoprobe	A photodynamic and photochemotherapeutic platinum-iridium charge-transfer conjugate for anticancer therapy Huayun Shi , Oliver W. L. Carter , Fortuna Ponte , Cinzia Imberti , Miguel A. Gomez-Gonzalez , Fernando Cacho-Nerin , Paul D. Quinn , Julia E. Parker , Emilia Sicilia , Huaiyi Huang , Peter J. Sadler Angewandte Chemie International Edition 12 DOI: 10.1002/anie.202400476 Diamond Proposal Number(s): [27852] Open Access Show Abstract ▼ Abstract: The novel hetero-dinuclear complex trans,trans,trans-[PtIV(py)2(N3)2(OH)(μ-OOCCH2CH2CONHCH2-bpyMe)IrIII(ppy)2]Cl (Pt-Ir), exhibits charge transfer between the acceptor photochemotherapeutic Pt(IV) (Pt-OH) and donor photodynamic Ir(III) (Ir-NH2) fragments. It is stable in the dark, but undergoes photodecomposition more rapidly than the Pt(IV) parent complex (Pt-OH) to generate Pt(II) species, an azidyl radical and 1O2. The Ir(III)* excited state, formed after irradiation, can oxidise NADH to NAD⋅ radicals and NAD+. Pt-Ir is highly photocytotoxic towards cancer cells with a high photocytotoxicity index upon irradiation with blue light (465 nm, 4.8 mW/cm2), even with short light-exposure times (10–60 min). In contrast, the mononuclear Pt-OH and Ir-NH2 subunits and their simple mixture are much less potent. Cellular Pt accumulation was higher for Pt-Ir compared to Pt-OH. Irradiation of Pt-Ir in cancer cells damages nuclei and releases chromosomes. Synchrotron-XRF revealed ca. 4× higher levels of intracellular platinum compared to iridium in Pt-Ir treated cells under dark conditions. Luminescent Pt-Ir distributes over the whole cell and generates ROS and 1O2 within 1 h of irradiation. Iridium localises strongly in small compartments, suggestive of complex cleavage and excretion via recycling vesicles (e.g. lysosomes). The combination of PDT and PACT motifs in one molecule, provides Pt-Ir with a novel strategy for multimodal phototherapy.	Apr 2024
I14-Hard X-ray Nanoprobe	Structural and chemical properties of anion exchanged CsPb(Br(1-x)Clx)3 heterostructured perovskite nanowires imaged by nanofocused x-rays Lucas Atila Bernardes Marcal , Nils Lamers , Susanna Hammarberg , Zhaojun Zhang , Huaiyu Chen , Dmitry Dzhigaev , Miguel Gomez-Gonzalez , Julia Parker , Alexander Bjorling , Anders Mikkelsen , Jesper Wallentin Nanotechnology DOI: 10.1088/1361-6528/ad355c Diamond Proposal Number(s): [25924] Open Access Show Abstract ▼ Abstract: Over the last years metal halide perovskites have demonstrated remarkable potential for integration in light emitting devices. Heterostructures allow for tunable bandgap depending on the local anion composition, crucial for optoelectronic devices, but local structural effects of anion exchange in single crystals is not fully understood. Here, we investigate how the anion exchange of CsPbBr3 nanowires fully and locally exposed to HCl vapor affects the local crystal structure, using nanofocused x-rays. We study the nanoscale composition and crystal structure as function of HCl exposure time and demonstrate the correlation of anion exchange with changes in the lattice parameter. The local composition was measured by x-ray fluorescence and x-ray diffraction, with general agreement of both methods but with much less variation using latter. The heterostructured nanowires exhibit unintentional gradients in composition, both axially and radially. Ferroelastic domains are observed for all HCl exposure times, and the magnitude of the lattice tilt decreases for higher Cl concentrations.	Mar 2024
I14-Hard X-ray Nanoprobe	An uneven distribution of strontium in the coccolithophore Scyphosphaera apsteinii revealed by nanoscale X-ray fluorescence tomography Jessica Walker , Hallam J. M. Greene , Yousef Moazzam , Paul D. Quinn , Julia E. Parker , Gerald Langer Environmental Science: Processes & Impacts 3 DOI: 10.1039/D3EM00509G Diamond Proposal Number(s): [31325] Open Access Show Abstract ▼ Abstract: Coccolithophores are biogeochemically and ecologically important phytoplankton that produce a composite calcium carbonate-based exoskeleton – the coccosphere – comprised of individual platelets, known as coccoliths. Coccoliths are stunning examples of biomineralization; their formation featuring exceptional control over both biomineral chemistry and shape. Understanding how coccoliths are formed requires information about minor element distribution and chemical environment. Here, the first high-resolution 3D synchrotron X-ray fluorescence (XRF) mapping of a coccolith is presented, showing that the lopadoliths of Scyphosphaera apsteinii display stripes of different Sr concentration. The presence of Sr stripes is unaffected by elevated Sr in the culture medium, macro-nutrient concentration, and light intensity, indicating that the observed stripiness is an expression of the fundamental coccolith formation process in this species. Current Sr fractionation models, by contrast, predict an even Sr distribution and will have to be modified to account for this stripiness. Additionally, nano-XANES analyses show that Sr resides in a Ca site in the calcite lattice in both high and low Sr stripes, confirming a central assumption of current Sr fractionation models.	Feb 2024
I11-High Resolution Powder Diffraction	Project M: investigating the effect of additives on calcium carbonate crystallisation through a school citizen science program Claire A. Murray , Project M Scientists , Laura Holland , Rebecca O'Brien , Alice Richards , Annabelle Baker , Mark Basham , David Bond , Leigh D. Connor , Sarah J. Day , Jacob Filik , Stuart Fisher , Peter Holloway , Karl Levik , Ronaldo Mercado , Jonathan Potter , Chiu C. Tang , Stephen P. Thompson , Julia E. Parker Crystengcomm 50 DOI: 10.1039/D3CE01173A Diamond Proposal Number(s): [15723] Open Access Show Abstract ▼ Abstract: Calcite and vaterite crystallisation is strongly influenced by the presence of additives during the reaction process, as demonstrated by organic molecules in biogenic calcium carbonate formation. The effect of additives on the lattice parameters of calcite and vaterite in syntheses are frequently reported, but only as discrete studies discussing a single polymorph. The intertwined nature of these polymorphs, due to their shared reaction pathway, is rarely discussed. In this work we report the results of a large scale citizen science project to explore the influence of amino acids and related additives on both polymorphs, highlighting their differences and commonalities in terms of the effect on the lattice parameters and polymorph selectivity.	Jan 2024
I11-High Resolution Powder Diffraction	Forming bonds between molecules and communities through Project M Claire Murray , Laura Holland , Rebecca O'Brien , Julia E. Parker Frontiers In Communication 8 DOI: 10.3389/fcomm.2023.1229616 Diamond Proposal Number(s): [15723] Open Access Show Abstract ▼ Abstract: Calcium carbonate is a compound that is well-recognized and very prevalent in daily life e.g., chalk, mussel shells and limescale. However, scientists still have many questions about its formation mechanisms, the different crystal forms it takes, and how we can control and direct this formation to produce this material with different properties. Project M was a chemistry citizen science project for UK secondary schools exploring the synthesis of samples of calcium carbonate under different reaction conditions and analyzing them at Beamline I11, an X-ray diffraction laboratory at the Diamond Light Source synchrotron. Science communication played a crucial role in the success of the project, connecting different communities to the science and creating unique opportunities to center and empower the Project M Scientists.	Nov 2023
I14-Hard X-ray Nanoprobe	Toward understanding the environmental risks of combined microplastics/nanomaterials exposures: unveiling ZnO transformations after adsorption onto polystyrene microplastics in environmental solutions Miguel A. Gomez-Gonzalez , Tatiana Da Silva-Ferreira , Nathaniel Clark , Robert Clough , Paul D. Quinn , Julia E. Parker Global Challenges 10 DOI: 10.1002/gch2.202300036 Open Access Show Abstract ▼ Abstract: Over recent decades, there has been a dramatic increase in the manufacture of engineered nanomaterials, which has inevitably led to their environmental release. Zinc oxide (ZnO) is among the more abundant nanomaterial manufactured due to its advantageous properties, used for piezoelectric, semiconducting, and antibacterial purposes. Plastic waste is ubiquitous and may break down or delaminate into smaller microplastics, leaving open the question of whether these small polymers may alter the fate of ZnO through adsorption within aquatic media (tap-water and seawater). Here, scanning electron microscopy analysis confirms the effective Zn nano/microstructures adsorption onto polystyrene surfaces after only 24-h incubation in the aquatic media. After pre-aging the nanomaterials for 7-days in different environmental media, nanoprobe X-ray absorption near-edge spectroscopy analysis reveals significant ZnO transformation toward Zn-sulfide and Zn-phosphate. The interaction between a commercial ZnO-based sunscreen with polystyrene and a cleanser consumer containing microbeads with ZnO nanomaterials is also studied, revealing the adsorption of transformed Zn-species in the microplastics surfaces, highlighting the environmental relevancy of this work. Understanding the structural and functional impacts of the microplastics/ZnO complexes, and how they evolve, will provide insights into their chemical nature, stability, transformations, and fate, which is key to predicting their bioreactivity in the environment.	Jul 2023
E01-JEM ARM 200CF I08-1-Soft X-ray Ptychography I13-2-Diamond Manchester Imaging I14-Hard X-ray Nanoprobe I18-Microfocus Spectroscopy	Multi-resolution correlative ultrastructural and chemical analysis of carious enamel by scanning microscopy and tomographic imaging Cyril Besnard , Ali Marie , Sisini Sasidharan , Petr Buček , Jessica M. Walker , Julia E. Parker , Matthew C. Spink , Robert A. Harper , Shashidhara Marathe , Kaz Wanelik , Thomas E. J. Moxham , Enrico Salvati , Konstantin Ignatyev , Michal M. Klosowski , Richard M. Shelton , Gabriel Landini , Alexander M. Korsunsky Acs Applied Materials & Interfaces 10 DOI: 10.1021/acsami.3c08031 Diamond Proposal Number(s): [27749, 30684, 30691, 31005, 29256, 23873] Open Access Show Abstract ▼ Abstract: Caries, a major global disease associated with dental enamel demineralization, remains insufficiently understood to devise effective prevention or minimally invasive treatment. Understanding the ultrastructural changes in enamel is hampered by a lack of nanoscale characterization of the chemical spatial distributions within the dental tissue. This leads to the requirement to develop techniques based on various characterization methods. The purpose of the present study is to demonstrate the strength of analytic methods using a correlative technique on a single sample of human dental enamel as a specific case study to test the accuracy of techniques to compare regions in enamel. The science of the different techniques is integrated to genuinely study the enamel. The hierarchical structures within carious tissue were mapped using the combination of focused ion beam scanning electron microscopy with synchrotron X-ray tomography. The chemical changes were studied using scanning X-ray fluorescence (XRF) and X-ray wide-angle and small-angle scattering using a beam size below 80 nm for ångström and nanometer length scales. The analysis of XRF intensity gradients revealed subtle variations of Ca intensity in carious samples in comparison with those of normal mature enamel. In addition, the pathways for enamel rod demineralization were studied using X-ray ptychography. The results show the chemical and structural modification in carious enamel with differing locations. These results reinforce the need for multi-modal approaches to nanoscale analysis in complex hierarchically structured materials to interpret the changes of materials. The approach establishes a meticulous correlative characterization platform for the analysis of biomineralized tissues at the nanoscale, which adds confidence in the interpretation of the results and time-saving imaging techniques. The protocol demonstrated here using the dental tissue sample can be applied to other samples for statistical study and the investigation of nanoscale structural changes. The information gathered from the combination of methods could not be obtained with traditional individual techniques.	Jul 2023
I14-Hard X-ray Nanoprobe	An in situ liquid environment for synchrotron hard X-ray nanoprobe microscopy Gea T. Van De Kerkhof , Jessica M. Walker , Surabhi Agrawal , Stuart M. Clarke , Mobbassar H. Sk , Dominic J. Craske , Robert Lindsay , Michael Dowhyj , Ayomide Osundare , Manfred E. Schuster , Julia E. Parker Materials At High Temperatures DOI: 10.1080/09603409.2023.2213579 Diamond Proposal Number(s): [28835] Open Access Show Abstract ▼ Abstract: Studying chemical reactions in an environment that closely mimics the system’s natural operating conditions can offer crucial insights into dynamic oxidation processes. Transmission Electron Microscopes (TEMs) and X-ray Nanoprobes allow the use of imaging and spectroscopy to access nanoscale chemical and structural information about these processes. However, the controlled operating conditions and constraints make the design and implementation of in situ sample environments challenging. Here, we outline the setup of an in situ liquid sample environment for the Hard X-ray Nanoprobe beamline (I14) at Diamond Light Source. The liquid environment allows for the imaging and spectroscopic analysis of samples exposed to liquid flow, with heating up to 80℃. The capability is demonstrated with an example experiment studying iron corrosion. The design of the sample cell offers the prospect of combining X-ray and electron microscopy for the in situ multi-length scale imaging and spectroscopy of samples in liquid.	May 2023

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