I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[22346, 21697]
Open Access
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.
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Dec 2021
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I13-1-Coherence
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Diamond Proposal Number(s):
[21767]
Open Access
Abstract: X-ray ptychography and X-ray fluorescence are complementary nanoscale imaging techniques, providing structural and elemental information, respectively. Both methods acquire data by scanning a localized beam across the sample. X-ray ptychography processes the transmission signal of a coherent illumination interacting with the sample, to produce images with a resolution finer than the illumination spot and step size. By enlarging both the spot and the step size, the technique can cover extended regions efficiently. X-ray fluorescence records the emitted spectra as the sample is scanned through the localized beam and its spatial resolution is limited by the spot and step size. The requisites for fast ptychography and high-resolution fluorescence appear incompatible. Here, a novel scheme that mitigates the difference in requirements is proposed. The method makes use of two probes of different sizes at the sample, generated by using two different energies for the probes and chromatic focusing optics. The different probe sizes allow to reduce the number of acquisition steps for the joint fluorescence–ptychography scan compared with a standard single beam scan, while imaging the same field of view. The new method is demonstrated experimentally using two undulator harmonics, a Fresnel zone plate and an energy discriminating photon counting detector.
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Nov 2021
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[20611]
Open Access
Abstract: The complex flow within the molten metallic pool, during advanced manufacturing and joining processes such as welding and additive manufacturing, directly affects the performance of the final components; through the generation of various microstructures and strain gradients. Understanding of the flow within such melt pools can enhance the predictability of the final microstructures and therefore component performance. In situ synchrotron X-ray imaging is employed to observe and map the evolving flow patterns within gas tungsten arc weld pools using tracking particles. The experimentally observed flow patterns are compared with numerical simulations to gain additional insights on accurate predictability in relevance to the physical driving forces within the flow. The spatio-temporal distribution of the flow using the mapped data is analyzed by considering the evolution of driving forces acting throughout the weld pool. The results demonstrate quantitative benchmark flow mapping with confirmation of the overall mechanisms of weld pool flow.
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Nov 2021
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B18-Core EXAFS
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Diamond Proposal Number(s):
[7314, 8372, 9050]
Open Access
Abstract: Thanks to its insolubility, mineral dust is considered a stable proxy in polar ice cores. With this study we show that the Talos Dome ice core (TALDICE, Ross Sea sector of East Antarctica) displays evident and progressive signs of post-depositional processes affecting the mineral dust record below 1000 m deep. We apply a suite of established and cutting-edge techniques to investigate the properties of dust in TALDICE, ranging from concentration and grain size to elemental composition and Fe mineralogy. Results show that through acidic/oxidative weathering, the conditions of deep ice at Talos Dome promote the dissolution of specific minerals and the englacial formation of others, affecting primitive dust features. The expulsion of acidic atmospheric species from ice grains and their concentration in localized environments is likely the main process responsible for englacial reactions. Deep ice can be seen as a “geochemical reactor” capable of fostering complex reactions which involve both soluble and insoluble impurities. Fe-bearing minerals can efficiently help in exploring such transformations.
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Oct 2021
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B22-Multimode InfraRed imaging And Microspectroscopy
I14-Hard X-ray Nanoprobe
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Diamond Proposal Number(s):
[22298]
Abstract: Unwanted N2O formation is a problem that has been noted in selective catalytic reduction (SCR) where copper zeolite catalysts are utilized. With its immense global warming potential and long-term stability, elevated atmospheric N2O has already been identified as a future challenge in the war on climate change. This paper explores the phenomenon of N2O formation during NH3-SCR over Cu-SSZ-13 catalysts, which are currently commercialized in automotive emissions control systems, and proposes a link between N2O production and the local copper environment found within the zeolite. To achieve this, a comparison is made between two Cu-SSZ-13 samples with different copper co-ordinations produced via different synthesis methods. A combination of synchrotron X-ray absorption near-edge spectroscopy, UV–vis, Raman, and density functional theory (DFT) is used to characterize the nature of copper species present within each sample. Synchrotron IR microspectroscopy is then used to compare their behavior during SCR under operando conditions and monitor the evolution of nitrate intermediates, which, along with further DFT, informs a mechanistic model for nitrate decomposition pathways. Increased N2O production is seen in the Cu-SSZ-13 sample postulated to contain a linear Cu species, providing an important correlation between the catalytic behavior of Cu-zeolites and the nature of their metal ion loading and speciation.
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Oct 2021
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I13-2-Diamond Manchester Imaging
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Birte
Hindenlang
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Anna
Gapeeva
,
Martina J.
Baum
,
Sören
Kaps
,
Lena M.
Saure
,
Florian
Rasch
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Jorg
Hammel
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Julian
Moosmann
,
Malte
Storm
,
Rainer
Adelung
,
Fabian
Schütt
,
Berit
Zeller-Plumhoff
Diamond Proposal Number(s):
[19205]
Open Access
Abstract: Tetrapodal zinc oxide (t-ZnO) is used to fabricate polymer composites for many different applications ranging from biomedicine to electronics. In recent times, macroscopic framework structures from t-ZnO have been used as a versatile sacrificial template for the synthesis of multi-scaled foam structures from different nanomaterials such as graphene, hexagonal boron nitride or gallium nitride. Many of these fabrication methods rely on wet-chemical coating processes using nanomaterial dispersions, leading to a strong interest in the actual coating mechanism and factors influencing it. Depending on the type of medium (e.g. solvent) used, different results regarding the homogeneity of the nanomaterial coating can be achieved. In order to understand how a medium influences the coating behavior, the evaporation process of water and ethanol is investigated in this work using in situ synchrotron radiation-based micro computed tomography (SRµCT). By employing propagation-based phase contrast imaging, both the t-ZnO network and the medium can be visualized. Thus, the evaporation process can be monitored non-destructively in three dimensions. This investigation showed that using a polar medium such as water leads to uniform evaporation and, by that, a homogeneous coating of the entire network.
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Oct 2021
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[13241]
Abstract: We propose a novel image analysis framework to automate analysis of X-ray micro-tomography images of sintering ceramics and glasses, using open-source toolkits and machine learning. Additive manufacturing (AM) of glasses and ceramics usually requires sintering of green bodies. Sintering causes shrinkage, which presents a challenge for controlling the metrology of the final architecture. Therefore, being able to monitor sintering in 3D over time (termed 4D) is important when developing new porous ceramics or glasses. Synchrotron X-ray tomographic imaging allows in situ, real-time capture of the sintering process at both micro and macro scales using a furnace rig, facilitating 4D quantitative analysis of the process. The proposed image analysis framework is capable of tracking and quantifying the densification of glass or ceramic particles within multiple volumes of interest (VOIs) along with structural changes over time using 4D image data. The framework is demonstrated by 4D quantitative analysis of bioactive glass ICIE16 within a 3D printed scaffold. Here, densification of glass particles within 3 VOIs were tracked and quantified along with diameter change of struts and inter-strut pore size over the 3D image series, delivering new insights on the sintering mechanism of ICIE16 bioactive glass particles in both micro and macro scales.
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Oct 2021
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[22627]
Abstract: Ductile cast irons (DCIs) are of increasing importance in the renewable energy and transportation sectors. The distribution and morphology of the graphite nodules, in particular the formation of degenerate features during solidification, dictate the mechanical performance of DCIs. In situ high-speed synchrotron X-ray tomography was used to capture the evolution of graphite nodules during solidification of DCI, including degenerate features and the effect of the carbon concentration field. The degeneration of nodules is observed to increase with re-melting cycles, which is attributed to Mg-loss. The dendritic primary austenite and carbon concentration gradients in the surrounding liquid phase were found to control nodule morphology by locally restricting and promoting growth.
A coupled diffusion-mechanical model was developed, confirming the experimentally informed hypothesis that protrusions form through liquation cracking of the austenite shell and subsequent localised growth. These results provide valuable insights into the solidification kinetics of cast irons, supporting the design of advanced alloys.
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Oct 2021
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I13-2-Diamond Manchester Imaging
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Diamond Proposal Number(s):
[19322]
Open Access
Abstract: Many soft tissues, such as the intervertebral disc (IVD), have a hierarchical fibrous composite structure which suffers from regional damage. We hypothesise that these tissue regions have distinct, inherent fibre structure and structural response upon loading. Here we used synchrotron computed tomography (sCT) to resolve collagen fibre bundles (∼5μm width) in 3D throughout an intact native rat lumbar IVD under increasing compressive load. Using intact samples meant that tissue boundaries (such as endplate-disc or nucleus-annulus) and residual strain were preserved; this is vital for characterising both the inherent structure and structural changes upon loading in tissue regions functioning in a near-native environment. Nano-scale displacement measurements along >10,000 individual fibres were tracked, and fibre orientation, curvature and strain changes were compared between the posterior-lateral region and the anterior region. These methods can be widely applied to other soft tissues, to identify fibre structures which cause tissue regions to be more susceptible to injury and degeneration. Our results demonstrate for the first time that highly-localised changes in fibre orientation, curvature and strain indicate differences in regional strain transfer and mechanical function (e.g. tissue compliance). This included decreased fibre reorientation at higher loads, specific tissue morphology which reduced capacity for flexibility and high strain at the disc-endplate boundary.
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Oct 2021
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I13-2-Diamond Manchester Imaging
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Aïcha
Ben Zemzem
,
Aline
Genevaux
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Amandine
Wahart
,
Andrew J.
Bodey
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Sébastien
Blaise
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Béatrice
Romier-Crouzet
,
Jessica
Jonquet
,
Camille
Bour
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Rémi
Cogranne
,
Pierre
Beauseroy
,
Manuel
Dauchez
,
Michael J.
Sherratt
,
Laurent
Debelle
,
Sébastien
Almagro
Diamond Proposal Number(s):
[12776]
Open Access
Abstract: The arterial wall consists of three concentric layers: intima, media, and adventitia. Beyond their resident cells, these layers are characterized by an extracellular matrix (ECM), which provides both biochemical and mechanical support. Elastin, the major component of arterial ECM, is present in the medial layer and organized in concentric elastic lamellae that confer resilience to the wall. We explored the arterial wall structures from C57Bl6 (control), db/db (diabetic), and ApoE−/− (atherogenic) mice aged 3 months using synchrotron X-ray computed microtomography on fixed and unstained tissues with a large image field (8 mm3). This approach combined a good resolution (0.83 µm/voxel), large 3D imaging field. and an excellent signal to noise ratio conferred by phase-contrast imaging. We determined from 2D virtual slices that the thickness of intramural ECM structures was comparable between strains but automated image analysis of the 3D arterial volumes revealed a lattice-like network within concentric elastic lamellae. We hypothesize that this network could play a role in arterial mechanics. This work demonstrates that phase-contrast synchrotron X-ray computed microtomography is a powerful technique which to characterize unstained soft tissues.
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Oct 2021
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