Search results for "Electron backscatter diffraction"
showing 10 items of 44 documents
Crystal structure of disordered nanocrystalline $\alpha^{II}$-quinacridone determined by electron diffraction
2016
CrystEngComm 18(4), 529 - 535(2016). doi:10.1039/C5CE01855B
Electron diffraction, X-ray powder diffraction and pair-distribution-function analyses to determine the crystal structures of Pigment Yellow 213, C23…
2009
The crystal structure of the nanocrystalline alpha phase of Pigment Yellow 213 (P.Y. 213) was solved by a combination of single-crystal electron diffraction and X-ray powder diffraction, despite the poor crystallinity of the material. The molecules form an efficient dense packing, which explains the observed insolubility and weather fastness of the pigment. The pair-distribution function (PDF) of the alpha phase is consistent with the determined crystal structure. The beta phase of P.Y. 213 shows even lower crystal quality, so extracting any structural information directly from the diffraction data is not possible. PDF analysis indicates the beta phase to have a columnar structure with a si…
Automated electron diffraction tomography - a new tool for nano crystal structure analysis
2011
Automated electron Diffraction Tomography (ADT) comprises an upcoming method for “ab intio” structure analysis of nano crystals. ADT allows fine sampling of the reciprocal space by sequential collection of electron diffraction patterns while tilting a nano crystal in fixed tilt steps around an arbitrary axis. Electron diffraction is collected in nano diffraction mode (NED) with a semi-parallel beam with a diameter down to 50 nm. For crystal tracking micro-probe STEM imaging is used. Full automation of the acquisition procedure allowed optimisation of the electron dose distribution and therefore analysis of highly beam sensitive samples. Cell parameters, space group and reflection intensitie…
Elucidating structural order and disorder phenomena in mullite-type Al4B2O9 by automated electron diffraction tomography
2017
The crystal structure and disorder phenomena of Al4B2O9, an aluminum borate from the mullite-type family, were studied using automated diffraction tomography (ADT), a recently established method for collection and analysis of electron diffraction data. Al4B2O9, prepared by sol-gel approach, crystallizes in the monoclinic space group C2/m. The ab initio structure determination based on three-dimensional electron diffraction data from single ordered crystals reveals that edge-connected AlO6 octahedra expanding along the b axis constitute the backbone. The ordered structure (A) was confirmed by TEM and HAADF-STEM images. Furthermore, disordered crystals with diffuse scattering along the b axis…
Towards automated diffraction tomography: Part I—Data acquisition
2007
Abstract The ultimate aim of electron diffraction data collection for structure analysis is to sample the reciprocal space as accurately as possible to obtain a high-quality data set for crystal structure determination. Besides a more precise lattice parameter determination, fine sampling is expected to deliver superior data on reflection intensities, which is crucial for subsequent structure analysis. Traditionally, three-dimensional (3D) diffraction data are collected by manually tilting a crystal around a selected crystallographic axis and recording a set of diffraction patterns (a tilt series) at various crystallographic zones. In a second step, diffraction data from these zones are com…
Ab Initio Structure Determination of Vaterite by Automated Electron Diffraction
2012
tion that is fundamental for understanding material properties. Still, a number of compounds have eluded such kinds of analysis because they are nanocrystalline, highly disordered, with strong pseudosymmetries or available only in small amounts in polyphasic or polymorphic systems. These materials are crystallographically intractable with conventional Xray or synchrotron radiation diffraction techniques. Single nanoparticles can be visualized by high-resolution transmission electron microscopy (HR-TEM) up to sub�ngstrom resolution, [2] but obtaining 3D information is still a difficult task, especially for highly beam-sensitive materials and crystal structures with long cell parameters. Elec…
Structure solution of zeolites by automated electron diffraction tomography - Impact and treatment of preferential orientation
2014
Abstract In this paper the reliability of structure solution of nano-crystalline porous compounds with preferred orientation based on automated electron diffraction tomography (ADT) is discussed. It will be shown that the limitations of the data acquisition geometry can be overcome by completing the missing diffraction data with additional diffraction information. Apart from different ways of sample preparation, data merging with either additional ADT data sets or intensities derived from X-ray powder diffraction comprise an effective way to improve the accuracy of the structure solution.
Applications of automated diffraction tomography (ADT) on nanocrystalline porous materials
2013
Abstract Many porous materials, both inorganic and hybrid organic–inorganic, can only be synthesized as nanocrystals. X-ray powder diffraction delivers one-dimensional data from the overall sample and is therefore often limited by peak overlap at low or medium resolution and by peak broadening. Thus, structure solution of materials with large unit cells and low symmetry, disorder or pseudosymmetry, or available only in polyphasic systems, turns out to be problematic or even impossible. Electron diffraction allows collecting three-dimensional structure information from nanocrystalline materials, but is traditionally biased by low completeness of the diffraction data, dynamical scattering and…
Study of plastic deformation modes in zirconium by color image analysis
2004
Abstract Twinning, as a deformation mode, is a complement to slip. This paper deals with the study from a qualitative point of view, as well as from a quantitative one. Besides techniques widely used in materials science studies such as electron backscattered diffraction (EBSD) or X-ray diffraction (XRD), colour image analysis technique are presented here. Its results manage to confirm or complete the ones obtained, thanks to others methods.
Application of delta recycling to electron automated diffraction tomography data from inorganic crystalline nanovolumes
2013
δ Recycling is a simple procedure for directly extracting phase information from Patterson-type functions [Rius (2012). Acta Cryst. A68, 399-400]. This new phasing method has a clear theoretical basis and was developed with ideal single-crystal X-ray diffraction data. On the other hand, introduction of the automated diffraction tomography (ADT) technique has represented a significant advance in electron diffraction data collection [Kolb et al. (2007). Ultramicroscopy, 107, 507-513]. When combined with precession electron diffraction, it delivers quasi-kinematical intensity data even for complex inorganic compounds, so that single-crystal diffraction data of nanometric volumes are now availa…