Discovery and Structure Determination of an Unusual Sulfide Telluride through an Effective Combination of TEM and Synchrotron Microdiffraction

Abstract

The structure elucidation of the novel sulfide telluride Pb8Sb8S15Te5 demonstrates a new versatile procedure that exploits the synergism of electron microscopy and synchrotron diffraction methods for accurate structure analyses of side-phases in heterogeneous microcrystalline samples. Suitable crystallites of unknown compounds can be identified by transmission electron microscopy and relocated and centered in a microfocused synchrotron beam by means of X-ray fluorescence scans. The refined structure model is then confirmed by simulating HRTEM images of the same crystallite. Pb8Sb8S15Te5 consists of chains of heterocubane-like units. Cation coordination polyhedra form unusually entwined chains of edge- and face-sharing bicapped trigonal prisms. The structure data are precise enough for bond-valence calculations, which confirm the disordered atom distribution. On this basis, optimization of physical properties becomes feasible.

Heterostructures of skutterudites and germanium antimony tellurides – structure analysis and thermoelectric properties of bulk samples

“…30). Thus, a discrete skutteruditetype crystallite in a polished and thinned slab cut from an ingot was selected by means of TEM.…”

Ba1.63La7.39Si11N23Cl0.42:Ce3+ – A Nitridosilicate Chloride with a Zeolite‐Like Structure

“…However, the use of microfocused synchrotron radiation has been shown to solve this problem efficiently, enabling high-quality data and structure refinements for very small crystallites. [24] In this article, the crystal structure of Ba 1 …”

Ammonothermal Synthesis of the Mixed‐Valence Nitrogen‐Rich Europium Tantalum Ruddlesden‐Popper Phase EuIIEuIII2Ta2N4O3

“…X‐ray diffraction data of Eu 3 Ta 2 N 4 O 3 were obtained by microfocus synchrotron diffraction (beamline ID11, ESRF, Grenoble) on a Huber diffractometer ( λ = 0.30996 Å) with a FReLoN2K CCD detector . A crystallite that had been pre‐characterized by TEM methods (see below) was used . Integration and empirical absorption correction was done with CrysAlis Pro .…”

“…The microscope was operated at 200 kV accelerating voltage. For evaluation of the TEM data, the following software was used: Digital Micrograph (measurement of d‐values from SAEDs), ProcessDiffraction7 (geometric calculations for SAED) and jEMS (SAED‐Simulations) , …”