Structure solution of zeolites by automated electron diffraction tomography – Impact and treatment of preferential orientation

2014 ◽  
Vol 189 ◽  
pp. 107-114 ◽  
Author(s):  
E. Mugnaioli ◽  
U. Kolb
Author(s):  
Mauro Gemmi ◽  
Arianna E. Lanza

3D electron diffraction is an emerging technique for the structural analysis of nanocrystals. The challenges that 3D electron diffraction has to face for providing reliable data for structure solution and the different ways of overcoming these challenges are described. The route from zone axis patterns towards 3D electron diffraction techniques such as precession-assisted electron diffraction tomography, rotation electron diffraction and continuous rotation is also discussed. Finally, the advantages of the new hybrid detectors with high sensitivity and fast readout are demonstrated with a proof of concept experiment of continuous rotation electron diffraction on a natrolite nanocrystal.


Author(s):  
Joke Hadermann ◽  
Artem M. Abakumov

The applicability of electron diffraction tomography to the structure solution and refinement of charged, discharged or cycled metal-ion battery positive electrode (cathode) materials is discussed in detail. As these materials are often only available in very small amounts as powders, the possibility of obtaining single-crystal data using electron diffraction tomography (EDT) provides unique access to crucial information complementary to X-ray diffraction, neutron diffraction and high-resolution transmission electron microscopy techniques. Using several examples, the ability of EDT to be used to detect lithium and refine its atomic position and occupancy, to solve the structure of materials ex situ at different states of charge and to obtain in situ data on structural changes occurring upon electrochemical cycling in liquid electrolyte is discussed.


2014 ◽  
Vol 53 (10) ◽  
pp. 5067-5072 ◽  
Author(s):  
Arnaud Mayence ◽  
Julien R. G. Navarro ◽  
Yanhang Ma ◽  
Osamu Terasaki ◽  
Lennart Bergström ◽  
...  

Author(s):  
Olesia Karakulina ◽  
Stanislav Fedotov ◽  
Vasiliy Sumanov ◽  
Oleg Drozhzhin ◽  
Nellie Khasanova ◽  
...  

2009 ◽  
Vol 1184 ◽  
Author(s):  
Ute Kolb ◽  
Tatiana Gorelik ◽  
Enrico Mugnaioli

AbstractThree-dimensional electron diffraction data was collected with our recently developed module for automated diffraction tomography and used to solve inorganic as well as organic crystal structures ab initio. The diffraction data, which covers nearly the full relevant reciprocal space, was collected in the standard nano electron diffraction mode as well as in combination with the precession technique and was subsequently processed with a newly developed automated diffraction analysis and processing software package. Non-precessed data turned out to be sufficient for ab initio structure solution by direct methods for simple crystal structures only, while precessed data allowed structure solution and refinement in all of the studied cases.


2009 ◽  
Vol 15 (S2) ◽  
pp. 738-739
Author(s):  
PA Midgley ◽  
A Eggeman ◽  
T White ◽  
E Bithell

Extended abstract of a paper presented at Microscopy and Microanalysis 2009 in Richmond, Virginia, USA, July 26 – July 30, 2009


2018 ◽  
Vol 4 (12) ◽  
pp. eaau6178 ◽  
Author(s):  
Péter Németh ◽  
Enrico Mugnaioli ◽  
Mauro Gemmi ◽  
György Czuppon ◽  
Attila Demény ◽  
...  

Despite its thermodynamical metastability at near-surface conditions, aragonite is widespread in marine and terrestrial sediments. It abundantly forms in living organisms, and its abiotic formation is favored in waters of a Mg2+/Ca2+ratio > 1.5. Here, we provide crystallographic evidence of a nanocrystalline CaCO3polymorph, which precipitates before aragonite in a cave. The new phase, which we term monoclinic aragonite (mAra), is crystallographically related to ordinary, orthorhombic aragonite. Electron diffraction tomography combined with structure determination demonstrates that mAra has a layered aragonite structure, in which some carbonates can be replaced by hydroxyls and up to 10 atomic % of Mg can be incorporated. The diagnostic electron diffraction features of mAra are diffuse scattering and satellite reflections along aragonite {110}. Similar features have previously been reported—although unrecognized—from biogenic aragonite formed in stromatolites, mollusks, and cyanobacteria as well as from synthetic material. We propose that mAra is a widespread crystalline CaCO3that plays a hitherto unrecognized key role in metastable aragonite formation.


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