Reconstruction of Single-Grain Orientation Distribution Functions for Crystalline Materials

A fundamental imaging problem in microstructural analysis of metals is the reconstruction of local crystallographic orientations from X-ray diffraction measurements. This work deals with the computation of the 3D orientation distribution function for individual grains of the material in consideration. We present an iterative large-scale algorithm that uses preconditioned regularizing CGLS iterations with a stopping criterion based on the information available in the residual vectors

Revealing three-dimensional structure of individual colloidal crystal grain by coherent x-ray diffractive imaging

We present results of a coherent x-ray diffractive imaging experiment performed on a single colloidal crystal grain. The full three-dimensional (3D) reciprocal space map measured by an azimuthal rotational scan contained several orders of Bragg reflections together with the coherent interference signal between them. Applying the iterative phase retrieval approach, the 3D structure of the crystal grain was reconstructed and positions of individual colloidal particles were resolved. As a result, an exact stacking sequence of hexagonal close-packed layers including planar and linear defects were identified.Comment: 8 pages, 5 figure

Optimization of Al/AlOx/AlAl/AlO_x/Al-Layer Systems for Josephson Junctions from a Microstructure Point of View

$Al/AlO_x/Al$-layer systems are frequently used for Josephson junction-based superconducting devices. Although much work has been devoted to the optimization of the superconducting properties of these devices, systematic studies on influence of deposition conditions combined with structural analyses on the nanoscale are rare up to now. We have focused on the optimization of the structural properties of $Al/AlO_x/Al$-layer systems deposited on Si(111) substrates with a particular focus on the thickness homogeneity of the $AlO_x$-tunnel barrier. A standard high-vacuum electron-beam deposition system was used and the effect of substrate pretreatment, different Al-deposition temperatures and Al-deposition rates was studied. Transmission electron microscopy was applied to analyze the structural properties of the $Al/AlO_x/Al$-layer systems to determine the thickness homogeneity of the $AlO_x$ layer, grain size distribution in the Al layers, Al-grain boundary types and the morphology of the $Al/AlO_x$ interface. We show that the structural properties of the lower Al layer are decisive for the structural quality of the whole $Al/AlO_x/Al$-layer system. Optimum conditions yield an epitaxial Al(111) layer on a Si(111) substrate with an Al-layer thickness variation of only 1.6 nm over more than 10 $\mu m$ and large lateral grain sizes up to 1 $\mu m$. Thickness fluctuations of the $AlO_x$-tunnel barrier are minimized on such an Al layer which is essential for the homogeneity of the tunnel current. Systematic variation of the Al-deposition rate and deposition temperature allows to develop an understanding of the growth mechanisms

py4DSTEM: a software package for multimodal analysis of four-dimensional scanning transmission electron microscopy datasets

Scanning transmission electron microscopy (STEM) allows for imaging, diffraction, and spectroscopy of materials on length scales ranging from microns to atoms. By using a high-speed, direct electron detector, it is now possible to record a full 2D image of the diffracted electron beam at each probe position, typically a 2D grid of probe positions. These 4D-STEM datasets are rich in information, including signatures of the local structure, orientation, deformation, electromagnetic fields and other sample-dependent properties. However, extracting this information requires complex analysis pipelines, from data wrangling to calibration to analysis to visualization, all while maintaining robustness against imaging distortions and artifacts. In this paper, we present py4DSTEM, an analysis toolkit for measuring material properties from 4D-STEM datasets, written in the Python language and released with an open source license. We describe the algorithmic steps for dataset calibration and various 4D-STEM property measurements in detail, and present results from several experimental datasets. We have also implemented a simple and universal file format appropriate for electron microscopy data in py4DSTEM, which uses the open source HDF5 standard. We hope this tool will benefit the research community, helps to move the developing standards for data and computational methods in electron microscopy, and invite the community to contribute to this ongoing, fully open-source project

Line Defects in Molybdenum Disulfide Layers

Layered molecular materials and especially MoS2 are already accepted as promising candidates for nanoelectronics. In contrast to the bulk material, the observed electron mobility in single-layer MoS2 is unexpectedly low. Here we reveal the occurrence of intrinsic defects in MoS2 layers, known as inversion domains, where the layer changes its direction through a line defect. The line defects are observed experimentally by atomic resolution TEM. The structures were modeled and the stability and electronic properties of the defects were calculated using quantum-mechanical calculations based on the Density-Functional Tight-Binding method. The results of these calculations indicate the occurrence of new states within the band gap of the semiconducting MoS2. The most stable non-stoichiometric defect structures are observed experimentally, one of which contains metallic Mo-Mo bonds and another one bridging S atoms

Time-of-Flight Three Dimensional Neutron Diffraction in Transmission Mode for Mapping Crystal Grain Structures

The physical properties of polycrystalline materials depend on their microstructure, which is the nano-to centimeter scale arrangement of phases and defects in their interior. Such microstructure depends on the shape, crystallographic phase and orientation, and interfacing of the grains constituting the material. This article presents a new non-destructive 3D technique to study centimeter-sized bulk samples with a spatial resolution of hundred micrometers: time-of-flight three-dimensional neutron diffraction (ToF 3DND). Compared to existing analogous X-ray diffraction techniques, ToF 3DND enables studies of samples that can be both larger in size and made of heavier elements. Moreover, ToF 3DND facilitates the use of complicated sample environments. The basic ToF 3DND setup, utilizing an imaging detector with high spatial and temporal resolution, can easily be implemented at a time-of-flight neutron beamline. The technique was developed and tested with data collected at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Complex (J-PARC) for an iron sample. We successfully reconstructed the shape of 108 grains and developed an indexing procedure. The reconstruction algorithms have been validated by reconstructing two stacked Co-Ni-Ga single crystals, and by comparison with a grain map obtained by post-mortem electron backscatter diffraction (EBSD)