A new layered mesoporous
Zr-MOF of composition [Zr30O20(OH)26(OAc)18L18]
was synthesized by employing 5-acetamidoisophthalic acid (H2L) using acetic acid as the solvent. The new MOF, denoted
as CAU-45, exhibits a honeycomb structure of stacked layers which
comprise both hexa- and dodecanucelar zirconium clusters. Its structure
was solved from submicrometer-sized crystals by continuous rotation
electron diffraction (cRED). Liquid phase exfoliation and size selection
were successfully performed on the material.
Highly porous three-dimensional Al- and Ga-MOFs with radical catecholate linker molecules were synthesized and characterized by electron diffraction, molecular simulation, Rietveld refinement and N2 sorption measurements.
Cover: The small cross section in the lower right part shows inter-and/or transcrystalline cracks in the wall sheet of a 20 years old swimming pool made of stainless steel. The samples tested as well as the visual on-site inspection revealed pitting at the outer surface of the wall sheet (see large photograph) which initiated stress corrosion cracking. The main cause for the pitting was not an unsuitable material but the environmental conditions at the outer surface enabling accumulation of chloride ions. (Copyright: BAM) Heat tints on stainless steels are known to have a detrimental effect on the corrosion resistance of the welded joints. In this article, a relation between the level of discolouration, thickness, composition and corrosion resistance has been done. Scanning vibrating electrode technique demonstrated that heat tints dissolve electrochemically and pickling is the only post-weld cleaning technique that removes the anodic activity over the welded joint.
Three-dimensional electron diffraction (3D ED)/microcrystal electron diffraction (MicroED) techniques are gaining in popularity. However, the data processing often does not fit existing graphical user interface software, instead requiring the use of the terminal or scripting. Scipion-ED, described in this article, provides a graphical user interface and extendable framework for processing of 3D ED/MicroED data. An illustrative project is described, in which multiple 3D ED/MicroED data sets collected on tetragonal lysozyme were processed with DIALS through the Scipion-ED interface. The ability to resolve unmodelled features in the electrostatic potential map was compared between three strategies for merging data sets.
The Timepix detector is a hybrid electron detector with counting capability dedicated for recording electron diffraction patterns. The detector has ultra-fast read-out (8.3 ms, up to 120 frames/s), high sensitivity and theoretically zero noise. These are especially useful for collecting 3D electron diffraction data from beam sensitive materials for structural analysis, with methods such as Rotation Electron Diffraction (RED), Automated Diffraction Tomography (ADT) and continuous rotation being developed. In recent years many complex unknown structures were solved using 3D electron diffraction methods. Such structures include zeolites, metal-organic frameworks (MOFs), organic compounds and open-framework germanates. The mentioned 3D electron diffraction methods all involve reconstructing the 3D reciprocal space from a number of diffraction patterns taken at different angles. This requires accurate intensities to be recorded for both strong and weak Bragg spots to give an accurate reconstruction, and the exposure time for each image must be low. In order to collect meaningful electron diffraction data, each pixel of the detector has to behave linearly up to its counting limit (11800) against the exposure time and the number of incident electrons. Thus, we tested the behaviour of a Timepix detector installed on a JEOL 2100 TEM with LaB6 filament. We compared the same set of strong, medium and weak Bragg spots in diffraction patterns collected using exposure time ranging from 1 ms to 262144 ms with a step size of 2n ms (where n equals to 1,2,3…). It was found that the measured intensities of the Bragg spot are linearly proportional to the exposure time between 25 and 11500 counts per pixel. Furthermore, the slopes of the linear region of the measured intensities from the strong, medium and weak Bragg spots against the exposure time were very similar. These results indicate the linear behaviour of the Timepix detector against both the exposure time and the number of incident electron within the dynamical range of the detector. Therefore, electron diffraction patterns collected by the Timepix detector can be quantitatively used for structural analysis by electron crystallography.
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