Cinthia Antunes Corrêa

Structure refinement using precession electron diffraction tomography and dynamical diffraction: theory and implementation.

Accurate structure refinement from electron-diffraction data is not possible without taking the dynamical-diffraction effects into account. A complete three-dimensional model of the structure can be obtained only from a sufficiently complete three-dimensional data set. In this work a method is presented for crystal structure refinement from the data obtained by electron diffraction tomography, possibly combined with precession electron diffraction. The principle of the method is identical to that used in X-ray crystallography: data are collected in a series of small tilt steps around a rotation axis, then intensities are integrated and the structure is optimized by least-squares refinement against the integrated intensities. In the dynamical theory of diffraction, the reflection intensities exhibit a complicated relationship to the orientation and thickness of the crystal as well as to structure factors of other reflections. This complication requires the introduction of several special parameters in the procedure. The method was implemented in the freely available crystallographic computing system Jana2006.

Structure refinement using precession electron diffraction tomography and dynamical diffraction: tests on experimental data.

The recently published method for the structure refinement from three-dimensional precession electron diffraction data using dynamical diffraction theory [Palatinus et al. (2015). Acta Cryst. A71, 235-244] has been applied to a set of experimental data sets from five different samples - Ni2Si, PrVO3, kaolinite, orthopyroxene and mayenite. The data were measured on different instruments and with variable precession angles. For each sample a reliable reference structure was available. A large series of tests revealed that the method provides structure models with an average error in atomic positions typically between 0.01 and 0.02 Å. The obtained structure models are significantly more accurate than models obtained by refinement using kinematical approximation for the calculation of model intensities. The method also allows a reliable determination of site occupancies and determination of absolute structure. Based on the extensive tests, an optimal set of the parameters for the method is proposed.

Silicene-terminated surface of calcium and strontium disilicides: properties and comparison with bulk structures by computational methods

Abstract The bulk and surface structures of calcium and strontium disilicides are investigated by computational methods using density functional theory. The investigated structures are R6, R3 and P1-CaSi2 and P1-SrSi2. The investigated properties are the cleavage energy at the silicene sheet, buckling of the bulk and surface silicene layers, charge transfer from calcium to silicon, band structure of bulk and surface-terminated structures and adsorption energies on H atoms and H2 molecules on the silicene-terminated surface of the R3 phase. The cleavage energy at the silicene surface is low in all cases. Structures P1-CaSi2 and R3-CaSi2 contain silicene sheets with different coordination to Ca, while R6-CaSi2 contains both types of the sheets. It is shown that the properties of the two types of silicene-like sheets in R6-CaSi2 are similar to those of the corresponding sheets in P1-CaSi2 and R3-CaSi2, and the thermodynamically stable R6 phase is a good candidate for experimental investigation of silicene-terminated surface in calcium disilicide.

Phase transitions and crystal structures of η′′-Cu(3+x)Si and η′′′-Cu(3+x)Si

Phase transitions and crystal structures of η’’-Cu(3+x)Si and η’’’-Cu(3+x)Si Cinthia Antunes Correa1,2, Morgane Poupon1, Olivier Pérez2, Robert Král1, Petra Zemenová1, Jérôme Lecourt2, Jaromír Kopeček1, Petr Brázda1, Mariana Klementová1, Lukáš Palatinus1 1Department Of Structure Analysis Institute Of Physics Of The Czech Academy Of, Prague, Czech Republic, 2Department of Physics of Materials, Charles University in Prague, Ke Karlovu 5, Prague 2, Czechia E-mail: cinthiacac@gmail.com