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In this paper we propose a new joint model for the reconstruction of tomography data under limited angle sampling regimes. In many applications of Tomography, e.g. Electron Microscopy and Mammography, physical limitations on acquisition lead to regions of data which cannot be sampled. Depending on the severity of the restriction, reconstructions can contain severe, characteristic, artefacts. Our model aims to address these artefacts by inpainting the missing data simultaneously with the reconstruction. Numerically, this problem naturally evolves to require the minimisation of a non-convex and non-smooth functional so we review recent work in this topic and extend results to fit an alternating (block) descent framework. We illustrate the effectiveness of this approach with numerical experiments on two synthetic datasets and one Electron Microscopy dataset., Comment: Revised manuscript accepted for publication in Inverse Problems

Advances in the production of two-dimensional (2D) materials such as graphene and MoS2 during the past two decades have spurred the search for other van der Waals materials with distinct functional properties. However, reducing the dimensionality of bulk van der Waals materials can lead to structural rearrangement and chemical degradation, especially in the presence of air. These challenges have slowed the progress of the discovery and analysis of chemically diverse 2D materials. Here, we provide a case study on the shear exfoliation of a class of wide band gap van der Waals materials termed II–VI layered hybrids (II–VI LHs) and show how reducing their dimension influences their structural and chemical stabilities. ZnSe(butylamine) and ZnSe(octylamine) are exfoliated, yielding shear-thinned material whose resistance toward degradation via oxidation is studied in depth by a variety of macro- and microscopic characterization techniques. Mechanical energy input, solvent–ligand interaction, and exposure to ambient conditions all play important roles in the stability of these materials. Our findings suggest that moderately coordinating alkylamine layers stabilize 2D materials that would otherwise degrade during exfoliation and exposure to air.

Recent demonstrations of melting in the metal–organic framework (MOF) family have created interest in the interfacial domain between inorganic glasses and amorphous organic polymers. The chemical and physical behaviour of porous hybrid liquids and glasses is of particular interest, though opportunities are limited by the inaccessible melting temperatures of many MOFs. Here, we show that the processing technique of flux melting, ‘borrowed’ from the inorganic domain, may be applied in order to melt ZIF-8, a material which does not possess an accessible liquid state in the pure form. Effectively, we employ the high-temperature liquid state of one MOF as a solvent for a secondary, non-melting MOF component. Differential scanning calorimetry, small- and wide-angle X-ray scattering, electron microscopy and X-ray total scattering techniques are used to show the flux melting of the crystalline component within the liquid. Gas adsorption and positron annihilation lifetime spectroscopy measurements show that this results in enhanced, accessible porosity to a range of guest molecules in the resultant flux melted MOF glass.

We present a new type of composite material involving the in situ immobilization of tin oxide nanoparticles (SnO2-NPs) within a monolithic metal-organic framework (MOF), the zeolitic imidazolate framework ZIF-8. SnO2@monoZIF-8 exploits the mechanical properties, structural resilience and high density of a monolithic MOF, whilst leveraging the photocatalytic action of the nanoparticles. The composite displays outstanding photocatalytic properties and represents a critical advance in the field of treating toxic effluents and a vital validation for commercial application. Crucially, full retention of catalytic activity was observed after 10 catalytic cycles.

Electron tomography bears promise for widespread determination of the three-dimensional arrangement of atoms in solids. However, it remains unclear whether methods successful for crystals are optimal for amorphous solids. Here, we explore the relative difficulty encountered in atomic-resolution tomography of crystalline and amorphous nanoparticles. We define an informational entropy to reveal the inherent importance of low-entropy zone-axis projections in the reconstruction of crystals. In turn, we propose considerations for optimal sampling for tomography of ordered and disordered materials.

Recent studies of single-atom catalysts open up the prospect of designing exceptionally active and environmentally efficient chemical processes. The stability and durability of such catalysts is governed by the strength with which the atoms are bound to their support and their diffusive behaviour. Here we use aberration-corrected STEM to image the diffusion of single copper adatoms on graphene oxide. We discover that individual atoms exhibit ano malous diffusion as a result of spatial and energetic disorder inherent in the support, and interpret the origins of this behaviour to develop a physical picture for the surface diffusion of single metal atoms.

An enhanced method to quantify energy dispersive spectra recorded in 3D with a scanning electron microscope (3D SEM-EDS) has been previously demonstrated. This paper presents an extension of this method using all the available X-ray lines generated by the beam. The extended method benefits from using high energy lines, that are more accurately quantified, and from using soft X-rays that are highly absorbed and thus more surface sensitive. The data used to assess the method are acquired with a dual beam FIB/SEM investigating a multi-element Ni-based superalloy. A high accelerating voltage, needed to excite the highest energy X-ray line, results in two available X-ray lines for several elements. The method shows an improved compositional quantification as well as an improved spatial resolution.

The paper concentrates on in situ transmission electron microscopy of nano-sized Mo and Nb clusters. In particular, this contribution presents challenges to control the microstructure in nanostructured materials via a relatively new approach, i.e. using a so-called nanocluster source. An important aspect is that the cluster size distribution is monodisperse and that the kinetic energy of the clusters during deposition can be varied. The deposited Mo clusters with sizes 5 nm or larger show a body-centered crystal (bcc) structure. The cubic clusters are self-assembled from smaller ones and forming distorted cubes of typical size 7.8 nm or larger. With reducing cluster size to

Operational stability is the main issue hindering the commercialisation of perovskite solar cells. Here, a long term light soaking test was performed on large area hybrid halide perovskite solar cells to investigate the morphological and chemical changes associated with the degradation of photovoltaic performance occurring within the devices. Using Scanning Transmission Electron Microscopy (STEM) in conjunction with EDX analysis on device cross sections, we observe the formation of gold clusters in the perovskite active layer as well as in the TiO2 mesoporous layer, and a severe degradation of the perovskite due to iodine migration into the hole transporter. All these phenomena are associated with a drastic drop of all the photovoltaic parameters. The use of advanced electron microscopy techniques and data processing provides new insights on the degradation pathways, directly correlating the nanoscale structure and chemistry to the macroscopic properties of hybrid perovskite devices.

Dusty olivine (olivine containing multiple sub-micrometer inclusions of metallic iron) in chondritic meteorites is considered an ideal carrier of paleomagnetic remanence, capable of maintaining a faithful record of pre-accretionary magnetization acquired during chondrule formation. Here we show how the magnetic architecture of a single dusty olivine grain from the Semarkona LL3.0 ordinary chondrite meteorite can be fully characterised in three dimensions, using a combination of Focussed-Ion-Beam nanotomography (FIB-nT), electron tomography and finite-element micromagnetic modelling. We present a three-dimensional (3D) volume reconstruction of a dusty olivine grain, obtained by selective milling through a region of interest in a series of sequential 20 nm slices, which are then imaged using scanning electron microscopy. The data provide a quantitative description of the iron particle ensemble, including the distribution of particle sizes, shapes, interparticle spacings and orientations. Iron particles are predominantly oblate ellipsoids with average radii 242 ± 94 nm by 199 ± 80 nm by 123 ± 58 nm. Using analytical TEM we observe that the particles nucleate on sub-grain boundaries and are loosely arranged in a series of sheets parallel to (001) of the olivine host. This is in agreement with the orientation data collected using the FIB-nT, and highlights how the underlying texture of the dusty olivine is crystallographically constrained by the olivine host. The shortest dimension of the particles is oriented normal to the sheets and their longest dimension is preferentially aligned within the sheets. Individual particle geometries are converted to a finite-element mesh and used to perform micromagnetic simulations. The majority of particles adopt a single vortex state, with ‘bulk’ spins that rotate around a central vortex core. We observed no particles, which are in a true single domain state. The results of the micromagnetic simulations challenge some pre-conceived ideas about the remanence carrying properties of vortex states. There is often not a simple predictive relationship between the major, intermediate and minor axes of the particles and the remanence vector imparted in different fields. Although the orientation of the vortex core is determined largely by the ellipsoidal geometry (i.e., parallel to the major axis for prolate ellipsoids and parallel to the minor axis for oblate ellipsoids), the core and remanence vectors can sometimes lie at very large (tens of degree) angles to the principal axes. The subtle details of the morphology can control the overall remanence state, leading in some cases to a dominant contribution from the bulk spins to the net remanence, with profound implications for predicting the anisotropy of the sample. The particles have very high switching fields (several hundred mT), demonstrating their high stability and suitability for paleointensity studies.

Recent paleomagnetic studies have constrained the strength and longevity of the magnetic field generated by the solar nebula, which has broad implications for the early evolution of the solar system. Paleomagnetic evidence was recorded by nanoscale iron inclusions in olivine crystals in the Semarkona LL 3.0 chondrite. These dusty olivines, have been shown to be credible carriers of ancient magnetic remanence. The small scale of the iron inclusions presents several challenges for defining their fundamental magnetic properties. Here we present the first correlative study of the response of these magnetic structures under applied laboratory fields. Results show that the majority of particles are in a single‐vortex state and exhibit stable magnetic behavior in applied fields up to 200 mT. Experimental observations using Lorentz microscopy and magnetic transmission X‐ray microscopy are shown to compare well with the results of finite‐element micromagnetic simulations derived from 3D models of the particles obtained using electron tomography. This correlative approach may be used to characterize the fundamental magnetic behavior of many terrestrial and extraterrestrial paleomagnetic carriers in the single‐ to multi‐vortex size range, which represent the vast majority of stable magnetic carriers in rocks and meteorites.

In this paper we propose a new joint model for the reconstruction of tomography data under limited angle sampling regimes. In many applications of Tomography, e.g. Electron Microscopy and Mammography, physical limitations on acquisition lead to regions of data which cannot be sampled. Depending on the severity of the restriction, reconstructions can contain severe, characteristic, artefacts. Our model aims to address these artefacts by inpainting the missing data simultaneously with the reconstruction. Numerically, this problem naturally evolves to require the minimisation of a non-convex and non-smooth functional so we review recent work in this topic and extend results to fit an alternating (block) descent framework. We illustrate the effectiveness of this approach with numerical experiments on two synthetic datasets and one Electron Microscopy dataset., Cantab Capital Institute for the Mathematics of Information PIHC innovation fund of the Technical Medical Centre of UT Dutch 4TU programme Precision Medicine Netherlands Organization for Scientific Research (NWO), project 639.073.506 Henslow Research Fellowship at Girton College, Cambridge Clare College Junior Research Fellowship