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

Instruments / Technical Area	Publication Details	Published
I13-2-Diamond Manchester Imaging	Evaluating the morphology of the degradation layer of pure magnesium via 3D imaging at resolutions below 40 nm Berit Zeller-Plumhoff , Daniel Laipple , Hanna Slominska , Kamila Iskhakova , Elena Longo , Alexander Hermann , Silja Flenner , Imke Greving , Malte Storm , Regine Willumeit-Römer Bioactive Materials 6, 4368 - 4376 DOI: 10.1016/j.bioactmat.2021.04.009 Diamond Proposal Number(s): [22346, 21697] Open Access Show Abstract ▼ Abstract: Magnesium is attractive for the application as a temporary bone implant due to its inherent biodegradability, non-toxicity and suitable mechanical properties. The degradation process of magnesium in physiological environments is complex and is thought to be a diffusion-limited transport problem. We use a multi-scale imaging approach using micro computed tomography and transmission X-ray microscopy (TXM) at resolutions below 40 nm. Thus, we are able to evaluate the nanoporosity of the degradation layer and infer its impact on the degradation process of pure magnesium in two physiological solutions. Magnesium samples were degraded in simulated body fluid (SBF) or Dulbecco's modified Eagle's medium (DMEM) with 10% fetal bovine serum (FBS) for one to four weeks. TXM reveals the three-dimensional interconnected pore network within the degradation layer for both solutions. The pore network morphology and degradation layer composition are similar for all samples. By contrast, the degradation layer thickness in samples degraded in SBF was significantly higher and more inhomogeneous than in DMEM+10%FBS. Distinct features could be observed within the degradation layer of samples degraded in SBF, suggesting the formation of microgalvanic cells, which are not present in samples degraded in DMEM+10%FBS. The results suggest that the nanoporosity of the degradation layer and the resulting ion diffusion processes therein have a limited influence on the overall degradation process. This indicates that the influence of organic components on the dampening of the degradation rate by the suppression of microgalvanic degradation is much greater in the present study.	Dec 2021
I12-JEEP: Joint Engineering, Environmental and Processing	Preferential wheat (Triticum aestivum. L cv. Fielder) root growth in different sized aggregates Tinashe Mawodza , Manoj Menon , Harriet Brooks , Oxana V. Magdysyuk , Genoveva Burca , Stuart Casson Soil And Tillage Research 212 DOI: 10.1016/j.still.2021.105054 Diamond Proposal Number(s): [22992] Show Abstract ▼ Abstract: Soil structure is one of the most important environmental factors affecting root architectural development and consequently plant yield. Understanding how plant roots respond to soils with variable soil structure is important as it enables soil management practices that promote optimal root growth. Many contemporary, non-invasive experiments investigating how plant root architecture responds to soil structural variations have often focused on compaction, often neglecting the role of soil aggregate size in determining root configuration. To better understand this, in this study, we used non-invasive neutron and X-Ray imaging to investigate how variable aggregate size affects the early root architectural establishment in wheat plants. Sandy loam soil derived macro-aggregates of two distinct sizes (0.25−0.5 and 2−4 mm) were used to infer the suitability of each aggregate size for use in wheat seedbeds. We also grew wheat seedlings in partitioned containers with the two different aggregate size classes filled side by side to establish whether there would be preferential growth of roots in either aggregate size class. Our results showed significantly increased root growth in the smaller 0.25−0.5 mm aggregates as compared to the larger 2−4 mm aggregates. This was mainly as a result of enhanced lateral root growth when the wheat plants were grown in the finer aggregates. On the other hand, coarser aggregates induced significantly increased seminal root axes which partially offset the differences in total root length between the two aggregate sizes. Plants growing in partitioned containers similarly indicated preferential root growth in smaller aggregate with an even more pronounced difference in root growth in the smaller aggregates. As inferred from our results, seedbeds dominated by smaller macro-aggregates (finer soil tilth) may be optimal to enhance wheat seedling root growth in sandy loam soils.	Aug 2021
I13-2-Diamond Manchester Imaging	The importance of particle dispersion in electrical treeing and breakdown in nano-filled epoxy resin Siyuan Chen , Simon Rowland , James Carr , Malte Storm , Kwang-Leong Choy , Adam J. Clancy International Journal Of Electrical Power & Energy Systems 129 DOI: 10.1016/j.ijepes.2021.106838 Diamond Proposal Number(s): [18215] Show Abstract ▼ Abstract: The addition of nano-fillers has been widely proposed as a method to enhance the dielectric properties of high voltage polymeric insulation, though there are mixed reports in the literature. Here the potential of silica nano-particles to extend the time to failure specifically through resistance to electrical tree growth in epoxy resin is determined. The benefit of silane treating the nano-particles before compounding is clearly established with regard to slowing tree growth and subsequent time to failure. The growth of trees in needle-plane samples is measured in the laboratory with loadings of 1, 3 and 5 wt% nano-filler. In all cases the average times to failure are extended, but silane treatment of the nano-particles prior to compounding yields much superior results. The emergence of a pronounced inception time before tree growth is also noted for the higher-filled, silane-treated cases. The average time to failure of silane-treated 5 wt% filled material was 28 times that of the unfilled resin. The improvement in performance between the nanocomposites with untreated and treated fillers is attributed to fewer agglomerations and improved dispersion of the filler in the treated cases. Measurements of Partial Discharge (PD) indicated significant differences in PD patterns during the growth of trees in the treated and untreated cases. This distinction may provide a quality control method for monitoring materials. In particular, long periods in which PDs were not measured were observed in the silane-treated cases. Visual imaging of tree growth in the unfilled material allowed the changing nature of the tree from fine to tree to dark tree to be observed as it grew. Corresponding PD measurements suggest the dark tree is gradually becoming conductive, and that growth of maximum PD measured is dependent on the relative rates of the growth of the tree and its carbonization. X-ray computer tomography identified significant differences in average tree channel diameters (a reduction from 2.8 µm to 2.0 µm for 1 wt% and 3 wt% cases). This implies that in addition to tree length changes, evaporated tree volumes also change and may explain the change in partial discharge characteristics observed.	Jul 2021
I13-2-Diamond Manchester Imaging	Enhanced near-infrared absorption for laser powder bed fusion using reduced graphene oxide Chu Lun Alex Leung , Iuliia Elizarova , Mark Isaacs , Shashidhara Marathe , Eduardo Saiz , Peter D. Lee Applied Materials Today 23 DOI: 10.1016/j.apmt.2021.101009 Diamond Proposal Number(s): [19354] Open Access Show Abstract ▼ Abstract: Laser powder bed fusion (LPBF) is a revolutionary manufacturing technology that fabricates parts with unparalleled complexity, layer-by-layer. However, there are limited choices of commercial powders for LPBF, constrained partly by the laser absorbance, an area that is not well investigated. Carbon additives are commonly used to promote near infra-red (NIR) absorbance of the powders but their efficiency is limited. Here, we combine operando synchrotron X-ray imaging with chemical characterisation techniques to elucidate the role of additives on NIR absorption, melt track and defect evolution mechanisms during LPBF. We employ a reduced graphene oxide (rGO) additive to enable LPBF of low NIR absorbance powder, SiO2, under systematic build conditions. This work successfully manufactured glass tracks with a high relative density (99.6%) and overhang features (> 5 mm long) without pre/post heat treatment. Compared to conventional carbon additives, the rGO increases the powder's NIR absorbance by ca. 3 times and decreases the warpage and porosity in LPBF glass tracks. Our approach will dramatically widen the palette of materials for laser processing and enable existing LPBF machines to process low absorbance powder, such as SiO2, using a NIR beam.	Jun 2021
	Protocol for image registration of correlative soft X-ray tomography and super-resolution structured illumination microscopy images Nina Vyas , Stephan Kunne , Thomas M. Fish , Ian M. Dobbie , Maria Harkiolaki , Perrine Paul-Gilloteaux Star Protocols 2 DOI: 10.1016/j.xpro.2021.100529 Open Access Show Abstract ▼ Abstract: Correlation of 3D images acquired on different microscopes can be a daunting prospect even for experienced users. This protocol describes steps for registration of images from soft X-ray absorption contrast imaging and super-resolution fluorescence imaging of hydrated biological materials at cryogenic temperatures. Although it is developed for data generated at synchrotron beamlines that offer the above combination of microscopies, it is applicable to all analogous imaging systems where the same area of a sample is examined using successive non-destructive imaging techniques.	Jun 2021
I14-Hard X-ray Nanoprobe	The Hard X-ray Nanoprobe beamline at Diamond Light Source Paul D. Quinn , Lucia Alianelli , Miguel Gomez-Gonzalez , David Mahoney , Fernando Cacho-Nerin , Andrew Peach , Julia E. Parker Journal Of Synchrotron Radiation 28 DOI: 10.1107/S1600577521002502 Open Access Show Abstract ▼ Abstract: The Hard X-ray Nanoprobe beamline, I14, at Diamond Light Source is a new facility for nanoscale microscopy. The beamline was designed with an emphasis on multi-modal analysis, providing elemental mapping, speciation mapping by XANES, structural phase mapping using nano-XRD and imaging through differential phase contrast and ptychography. The 185 m-long beamline operates over a 5 keV to 23 keV energy range providing a ≤50 nm beam size for routine user experiments and a flexible scanning system allowing fast acquisition. The beamline achieves robust and stable operation by imaging the source in the vertical direction and implementing horizontally deflecting primary optics and an overfilled secondary source in the horizontal direction. This paper describes the design considerations, optical layout, aspects of the hardware engineering and scanning system in operation as well as some examples illustrating the beamline performance.	May 2021
I12-JEEP: Joint Engineering, Environmental and Processing	Damage accumulation during high temperature fatigue of Ti/SiCf metal matrix composites under different stress amplitudes Ying Wang , Xu Xu , Wenxia Zhao , Nan Li , Samuel A. Mcdonald , Yuan Chai , Michael D. Atkinson , Katherine J. Dobson , Stefan Michalik , Yingwei Fan , Philip J. Withers , Xiaorong Zhou , Timothy L. Burnett Acta Materialia 16 DOI: 10.1016/j.actamat.2021.116976 Diamond Proposal Number(s): [20226] Open Access Show Abstract ▼ Abstract: The damage mechanisms and load redistribution taking place under high temperature (350°C), high cycle fatigue (HCF) of TC17 titanium alloy/unidirectional SiC fibre composites have been investigated in situ using synchrotron X-ray computed tomography (CT) and X-ray diffraction (XRD) under two stress amplitudes. The three-dimensional morphology of the fatigue crack and fibre fractures has been mapped by CT. At low stress amplitude, stable growth occurs with matrix cracking deflecting by 50-100 µm in height as it bypasses the bridging fibres. At higher stress amplitude, loading to the peak stress led to a burst of fibre fractures giving rise to rapid crack growth. Many of the fibre fractures occurred 50-300 µm above/below the matrix crack plane during rapid growth, contrary to that in the stable growth stage, leading to extensive fibre pull-out on the fracture surface. The changes in fibre loading, interfacial stress, and the extent of fibre-matrix debonding in the vicinity of the crack have been mapped over the fatigue cycle and after the rapid growth by XRD. The fibre/matrix interfacial sliding extends up to 600 µm (in the stable-growth zone) or 700 µm (in the rapid-growth zone) either side of the crack plane. The direction of interfacial shear stress reverses over the loading cycle, with the maximum frictional sliding stress reaching ∼55 MPa in both regimes. In accordance with previous studies, it is possible that a degradation in fibre strength at elevated temperature is responsible for bursts of fibre fracture and rapid crack growth under higher stress amplitude.	May 2021
I13-2-Diamond Manchester Imaging	3D analysis of enamel demineralisation in human dental caries using high-resolution, large field of view synchrotron X-ray micro-computed tomography Cyril Besnard , Robert A. Harper , Thomas E. J. Moxham , Jonathan D. James , Malte Storm , Enrico Salvati , Gabriel Landini , Richard M. Shelton , Alexander M. Korsunsky Materials Today Communications 392 DOI: 10.1016/j.mtcomm.2021.102418 Diamond Proposal Number(s): [20479] Open Access Show Abstract ▼ Abstract: We report major advances in the analysis of synchrotron 3D datasets acquired from human healthy and carious dental enamel. Synchrotron tomographic data for three human carious samples and a non-carious reference tooth sample were collected with the voxel size of 325 nm for a total volume of 815.4 × 815.4 × 685.4 μm3. The results were compared with conventional X-ray tomography, optical microscopy, and focused ion beam-scanning electron microscopy. Clear contrast was seen within demineralised enamel due to reduced mineral content using synchrotron tomography in comparison with conventional tomography. The features were found to correspond with the rod and inter-rod structures within prismatic enamel. 2D and 3D image segmentation allowed statistical quantification of important structural characteristics (such as the aspect ratio and the cross-sectional area of voids, as well as the demineralised volume fraction as a function of lesion depth). Whilst overall carious enamel predominantly displayed Type 1 etching pattern (preferential demineralisation of enamel rods), a transition between Type 2 (preferential inter-rod demineralisation) and Type 1 was identified within the same lesion for the first time. This study does not intend to give extensive results on the different lesions studied, but to illustrate a new method and its potential application.	May 2021
I14-Hard X-ray Nanoprobe	Nanoscale chemical imaging of nanoparticles under real‐world wastewater treatment conditions Miguel A. Gomez‐gonzalez , Mohamed A. Koronfel , Huw Pullin , Julia E. Parker , Paul D. Quinn , Maria D. Inverno , Thomas B. Scott , Fang Xie , Nikolaos Voulvoulis , Marian L. Yallop , Mary P. Ryan , Alexandra E. Porter Advanced Sustainable Systems 45 DOI: 10.1002/adsu.202100023 Diamond Proposal Number(s): [17784] Show Abstract ▼ Abstract: Understanding nanomaterial transformations within wastewater treatment plants is an important step to better predict their potential impact on the environment. Here, spatially resolved, in situ nano‐X‐ray fluorescence microscopy is applied to directly observe nanometer‐scale dissolution, morphological, and chemical evolution of individual and aggregated ZnO nanorods in complex “real‐world” conditions: influent water and primary sludge collected from a municipal wastewater system. A complete transformation of isolated ZnO nanorods into ZnS occurs after only 1 hour in influent water, but larger aggregates of the ZnO nanorods transform only partially, with small contributions of ZnS and Zn‐phosphate (Zn3(PO4)2) species, after 3 hours. Transformation of aggregates of the ZnO nanorods toward mixed ZnS, Zn adsorbed to Fe‐oxyhydroxides, and a large contribution of Zn3(PO4)2 phases are observed during their incubation in primary sludge for 3 hours. Discrete, isolated ZnO regions are imaged with unprecedented spatial resolution, revealing their incipient transformation toward Zn3(PO4)2. Passivation by transformation(s) into mixtures of less soluble phases may influence the subsequent bioreactivity of these nanomaterials. This work emphasizes the importance of imaging the nanoscale chemistry of mixtures of nanoparticles in highly complex, heterogeneous semi‐solid matrices for improved prediction of their impacts on treatment processes, and potential environmental toxicity following release.	May 2021
I23-Long wavelength MX	X-ray tomographic reconstruction and segmentation pipeline for the long-wavelength macromolecular crystallography beamline at Diamond Light Source Daniil Kazantsev , Ramona Duman , Armin Wagner , Vitaliy Mykhaylyk , Kazimir Wanelik , Mark Basham , Nicola Wadeson Journal Of Synchrotron Radiation 28 DOI: 10.1107/S1600577521003453 Open Access Show Abstract ▼ Abstract: In this paper a practical solution for the reconstruction and segmentation of low-contrast X-ray tomographic data of protein crystals from the long-wavelength macromolecular crystallography beamline I23 at Diamond Light Source is provided. The resulting segmented data will provide the path lengths through both diffracting and non-diffracting materials as basis for analytical absorption corrections for X-ray diffraction data taken in the same sample environment ahead of the tomography experiment. X-ray tomography data from protein crystals can be difficult to analyse due to very low or absent contrast between the different materials: the crystal, the sample holder and the surrounding mother liquor. The proposed data processing pipeline consists of two major sequential operations: model-based iterative reconstruction to improve contrast and minimize the influence of noise and artefacts, followed by segmentation. The segmentation aims to partition the reconstructed data into four phases: the crystal, mother liquor, loop and vacuum. In this study three different semi-automated segmentation methods are experimented with by using Gaussian mixture models, geodesic distance thresholding and a novel morphological method, RegionGrow, implemented specifically for the task. The complete reconstruction-segmentation pipeline is integrated into the MPI-based data analysis and reconstruction framework Savu, which is used to reduce computation time through parallelization across a computing cluster and makes the developed methods easily accessible.	May 2021

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