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Abstract: Hard dental tissues possess a complex hierarchical structure that is particularly evident in enamel, the most mineralised substance in the human body. Its complex and interlinked organisation at the Ångstrom (crystal lattice), nano-, micro-, and macro-scales is the result of evolutionary optimisation for mechanical and functional performance: hardness and stiffness, fracture toughness, thermal, and chemical resistance. Understanding the physical–chemical–structural relationships at each scale requires the application of appropriately sensitive and resolving probes. Synchrotron X-ray techniques offer the possibility to progress significantly beyond the capabilities of conventional laboratory instruments, i.e., X-ray diffractometers, and electron and atomic force microscopes. The last few decades have witnessed the accumulation of results obtained from X-ray scattering (diffraction), spectroscopy (including polarisation analysis), and imaging (including ptychography and tomography). The current article presents a multi-disciplinary review of nearly 40 years of discoveries and advancements, primarily pertaining to the study of enamel and its demineralisation (caries), but also linked to the investigations of other mineralised tissues such as dentine, bone, etc. The modelling approaches informed by these observations are also overviewed. The strategic aim of the present review was to identify and evaluate prospective avenues for analysing dental tissues and developing treatments and prophylaxis for improved dental health.

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Abstract: Indium selenides (InxSey) have been shown to retain several desirable properties, such as ferroelectricity, tunable photoluminescence through temperature-controlled phase changes, and high electron mobility when confined to two dimensions (2D). In this work we synthesize single-layer, ultrathin, subnanometer-wide InxSey by templated growth inside single-walled carbon nanotubes (SWCNTs). Despite the complex polymorphism of InxSey we show that the phase of the encapsulated material can be identified through comparison of experimental aberration-corrected transmission electron microscopy (AC-TEM) images and AC-TEM simulations of known structures of InxSey. We show that, by altering synthesis conditions, one of two different stoichiometries of sub-nm InxSey, namely InSe or β-In2Se3, can be prepared. Additionally, in situ AC-TEM heating experiments reveal that encapsulated β-In2Se3 undergoes a phase change to γ-In2Se3 above 400 °C. Further analysis of the encapsulated species is performed using X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), energy dispersive X-ray analysis (EDX), and Raman spectroscopy, corroborating the identities of the encapsulated species. These materials could provide a platform for ultrathin, subnanometer-wide phase-change nanoribbons with applications as nanoelectronic components.

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Abstract: The ability to control the in-plane magnetic anisotropy of a thin film is important for magnetic device applications. One way of accomplishing this task is by glancing angle deposition (GLAD). In this study, thin Co layers have been deposited using GLAD magnetron sputtering on MgO(001) and MgO(110) substrates. For Co films on MgO(001), the in-plane anisotropy direction can be directly controlled via the deposition angle. In contrast, for Co on MgO(110), the anisotropy due to the deposition angle is competing with the anisotropy induced by the substrate, while the growth parameters determine which contribution dominates. On the other hand, while on MgO(001) the deposition angle as well as the film thickness affect the strength of the Co in-plane anisotropy, no influence of these parameters on the magnetic properties is found for films on MgO(110).

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Abstract: We describe nNPipe for the automated analysis of morphologically diverse catalyst materials. Automated imaging routines and direct-electron detectors have enabled the collection of large data stacks over a wide range of sample positions at high temporal resolution. Simultaneously, traditional image analysis approaches are slow and hence unsuitable for large data stacks and consequently, researchers have progressively turned towards machine learning and deep learning approaches. Previous studies often detail work on morphologically uniform material systems with clearly discernible features, limited workable image sizes and training data that may be biased due to manual labelling. The nNPipe data-processing method consists of two standalone convolutional neural networks that were exclusively trained on multislice image simulations and enables fast analysis of 2048 × 2048 pixel images. Inference performance compared between idealised and real industrial catalytic samples and insights derived from subsequent data analysis are placed into the context of an automated imaging scenario.

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Abstract: Phyllosilicate minerals in the carbonaceous chondrites provide insights into processes in primitive parent bodies of the early Solar System. It is widely agreed that the CM- and CI-type carbonaceous chondrites underwent aqueous alteration on their parent bodies, resulting in phyllosilicate-rich matrices, where the dominant mineral phase is serpentine. There are many previous studies investigating phyllosilicate structure in carbonaceous chondrites, however, the presence of sulfur in these minerals and its effect on crystal lattice structure has not been studied in detail. We are investigating how the presence of sulfur (up to ≃9-10 wt% SO3) in serpentine phyllosilicate regions effects basal lattice spacing measurements of serpentine-like minerals in CM- and CI-type chondritic and related asteroidal material. Four specimens are being studied for this work: Winchcombe and Aguas Zarcas (CM-type), and Ryugu samples (A0058-C2001-08, A0104-00200502 and A0104-01700602) from Hayabusa2 and Ivuna (CI-type). All samples are TEM wafers. We have used a multi-technique approach to study the samples, with the E01 JEOL ARM200CF and E02 JEOL ARM300CF electron microscopes at the ePSIC facility at Diamond Light Source in Harwell, UK. EDS compositional data has been collected using the E01 microscope, whilst HRTEM and HAADF imaging data has been collected at E02. At E02 we are also applying a new 4D-STEM nano-diffraction technique in order to collect lattice spacing data to correlate with our other HRTEM results. Fe-K XANES analyses on Winchcombe and Ryugu have been carried out using the I18 microprobe and I14 hard x-ray nanoprobe respectively, also at Diamond Light Source, to constrain Fe3+/ΣFe. By combining these techniques we aim to better understand the physical and chemical structure of serpentine-like minerals in carbonaceous chondrites. Initial analyses have shown that sulfur presence in carbonaceous chondrite phyllosilicates reduces the basal lattice spacings of serpentine-like minerals. In these sulfur-bearing regions, we have been finding lattice spacings in the range ~0.60-0.74nm for the CM-type chondrites. For the CI-type, these range between ~0.65-0.76nm. Differences in the reduced lattice spacing ranges are likely related to the redox state of the sulfur. In Ryugu and other carbonaceous chondrites the sulfur appears reduced; its content in serpentine is low and we see FeS grains. Comparatively, in Winchcombe (and others) more of the sulfur seems to be in the serpentine structure. We can conclude that in serpentine-like minerals, the presence of sulfur appears to reduce basal lattice spacing values compared to the expected d-spacing value of 0.70nm for serpentine. Possible reasons for this include further investigations into the valency of the sulfur ions, the bonding environment within serpentine layers, and the location of sulfur in either the octa- or tetrahedral lattice sites.