Transfer of Individual Micro- and Nanoparticles for High- Precision 3D Analysis Using 360° Electron Tomography

A versatile approach is demonstrated, providing a general routine for an extensive and advanced 3D characterization of individually selected micro- and nanoparticles, enabling the combination of complementary and scale-bridging techniques. Quintessential to the method is the transfer of individual particles onto tailored tips using a conventional scanning electron microscope equipped with a suitable micromanipulator. The method enables a damage- and contamination-free preparation of freestanding particles. This is of significant importance for applications addressing the measurement of structural, physical, and chemical properties of specifically selected particles, such as 360° electron tomography, atom probe tomography, nano X-ray tomography, or optical near-field measurements. In this context, the method is demonstrated for 360° electron tomography of micro-/macroporous zeolite particles with sizes in the micrometer range and mesoporous alpha-hematite nanoparticles exhibiting sizes of 50–100 nm, including detailed pre- and postcharacterization on the nanoscale.“Deutsche Forschungsgemeinschaft” (DFG) within the framework of the SPP 1570 (project DFG SP 648/4-3 “3D analysis of complex pore structures using ET and high-resolution TEM”) and the research training group GRK 1896 (“In situ Microscopy with Electrons, X-rays and Scanning Probes”) as well as through the Cluster of Excellence “Engineering of Advanced Materials” at the Friedrich-Alexander-Universität Erlangen-Nürnberg (Germany)FIBJulian Losche

Geometric reconstruction methods for electron tomography

Electron tomography is becoming an increasingly important tool in materials science for studying the three-dimensional morphologies and chemical compositions of nanostructures. The image quality obtained by many current algorithms is seriously affected by the problems of missing wedge artefacts and nonlinear projection intensities due to diffraction effects. The former refers to the fact that data cannot be acquired over the full $180^\circ$ tilt range; the latter implies that for some orientations, crystalline structures can show strong contrast changes. To overcome these problems we introduce and discuss several algorithms from the mathematical fields of geometric and discrete tomography. The algorithms incorporate geometric prior knowledge (mainly convexity and homogeneity), which also in principle considerably reduces the number of tilt angles required. Results are discussed for the reconstruction of an InAs nanowire

A 3D Framework for Characterizing Microstructure Evolution of Li-Ion Batteries

Lithium-ion batteries are commonly found in many modern consumer devices, ranging from portable computers and mobile phones to hybrid- and fully-electric vehicles. While improving efficiencies and increasing reliabilities are of critical importance for increasing market adoption of the technology, research on these topics is, to date, largely restricted to empirical observations and computational simulations. In the present study, it is proposed to use the modern technique of X-ray microscopy to characterize a sample of commercial 18650 cylindrical Li-ion batteries in both their pristine and aged states. By coupling this approach with 3D and 4D data analysis techniques, the present study aimed to create a research framework for characterizing the microstructure evolution leading to capacity fade in a commercial battery. The results indicated the unique capabilities of the microscopy technique to observe the evolution of these batteries under aging conditions, successfully developing a workflow for future research studies

3D Coronal Density Reconstruction and Retrieving the Magnetic Field Structure during Solar Minimum

Measurement of the coronal magnetic field is a crucial ingredient in understanding the nature of solar coronal phenomena at all scales. We employed STEREO/COR1 data obtained during a deep minimum of solar activity in February 2008 (Carrington rotation CR 2066) to retrieve and analyze the three-dimensional (3D) coronal electron density in the range of heights from 1.5 to 4 Rsun using a tomography method. With this, we qualitatively deduced structures of the coronal magnetic field. The 3D electron density analysis is complemented by the 3D STEREO/EUVI emissivity in the 195 A band obtained by tomography for the same CR. A global 3D MHD model of the solar corona was used to relate the reconstructed 3D density and emissivity to open/closed magnetic field structures. We show that the density maximum locations can serve as an indicator of current sheet position, while the locations of the density gradient maximum can be a reliable indicator of coronal hole boundaries. We find that the magnetic field configuration during CR 2066 has a tendency to become radially open at heliocentric distances greater than 2.5 Rsun. We also find that the potential field model with a fixed source surface (PFSS) is inconsistent with the boundaries between the regions with open and closed magnetic field structures. This indicates that the assumption of the potential nature of the coronal global magnetic field is not satisfied even during the deep solar minimum. Results of our 3D density reconstruction will help to constrain solar coronal field models and test the accuracy of the magnetic field approximations for coronal modeling.Comment: Published in "Solar Physics

Linear chemically sensitive electron tomography using DualEELS and dictionary-based compressed sensing

We have investigated the use of DualEELS in elementally sensitive tilt series tomography in the scanning transmission electron microscope. A procedure is implemented using deconvolution to remove the effects of multiple scattering, followed by normalisation by the zero loss peak intensity. This is performed to produce a signal that is linearly dependent on the projected density of the element in each pixel. This method is compared with one that does not include deconvolution (although normalisation by the zero loss peak intensity is still performed). Additionaly, we compare the 3D reconstruction using a new compressed sensing algorithm, DLET, with the well-established SIRT algorithm. VC precipitates, which are extracted from a steel on a carbon replica, are used in this study. It is found that the use of this linear signal results in a very even density throughout the precipitates. However, when deconvolution is omitted, a slight density reduction is observed in the cores of the precipitates (a so-called cupping artefact). Additionally, it is clearly demonstrated that the 3D morphology is much better reproduced using the DLET algorithm, with very little elongation in the missing wedge direction. It is therefore concluded that reliable elementally sensitive tilt tomography using EELS requires the appropriate use of DualEELS together with a suitable reconstruction algorithm, such as the compressed sensing based reconstruction algorithm used here, to make the best use of the limited data volume and signal to noise inherent in core-loss EELS

High-resolution ab initio three-dimensional X-ray diffraction microscopy

Coherent X-ray diffraction microscopy is a method of imaging non-periodic isolated objects at resolutions only limited, in principle, by the largest scattering angles recorded. We demonstrate X-ray diffraction imaging with high resolution in all three dimensions, as determined by a quantitative analysis of the reconstructed volume images. These images are retrieved from the 3D diffraction data using no a priori knowledge about the shape or composition of the object, which has never before been demonstrated on a non-periodic object. We also construct 2D images of thick objects with infinite depth of focus (without loss of transverse spatial resolution). These methods can be used to image biological and materials science samples at high resolution using X-ray undulator radiation, and establishes the techniques to be used in atomic-resolution ultrafast imaging at X-ray free-electron laser sources.Comment: 22 pages, 11 figures, submitte

Review of the Synergies Between Computational Modeling and Experimental Characterization of Materials Across Length Scales

With the increasing interplay between experimental and computational approaches at multiple length scales, new research directions are emerging in materials science and computational mechanics. Such cooperative interactions find many applications in the development, characterization and design of complex material systems. This manuscript provides a broad and comprehensive overview of recent trends where predictive modeling capabilities are developed in conjunction with experiments and advanced characterization to gain a greater insight into structure-properties relationships and study various physical phenomena and mechanisms. The focus of this review is on the intersections of multiscale materials experiments and modeling relevant to the materials mechanics community. After a general discussion on the perspective from various communities, the article focuses on the latest experimental and theoretical opportunities. Emphasis is given to the role of experiments in multiscale models, including insights into how computations can be used as discovery tools for materials engineering, rather than to "simply" support experimental work. This is illustrated by examples from several application areas on structural materials. This manuscript ends with a discussion on some problems and open scientific questions that are being explored in order to advance this relatively new field of research.Comment: 25 pages, 11 figures, review article accepted for publication in J. Mater. Sc

Magnetization reversal and local switching fields of ferromagnetic Co/Pd microtubes with radial magnetization

Three-dimensional nanomagnetism is a rapidly growing field of research covering both noncollinear spin textures and curved magnetic geometries including microtubular structures. We spatially resolve the field-induced magnetization reversal of free-standing ferromagnetic microtubes utilizing multifrequency magnetic force microscopy (MFM). The microtubes are composed of Co/Pd multilayer films with perpendicular magnetic anisotropy that translates to an anisotropy with radial easy axis upon rolling-up. Simultaneously mapping the topography and the perpendicular magnetostatic force derivative, the relation between surface angle and local magnetization configuration is evaluated for a large number of locations with slopes exceeding 45 degrees. The angle-dependence of the switching field is concurrent with the Kondorsky model, i.e., the rolled-up nanomembrane behaves like a planar magnetic film with perpendicular anisotropy and a pinning dominated magnetization reversal. Additionally, we discuss methodological challenges when detecting magnetostatic force derivatives near steep surfaces