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A new film material capable of transforming UV radiation into visible light was obtained from a highly anisometric EuIII complex with organic ligands in a polymethylmethacrylate (PMMA) matrix and then structurally characterized. An important advantage of the synthesized complex is its good solubility in organic solvents such as dichloromethane, chloroform, THF, toluene, etc. The ligand environment (flexible alkyl and cyclohexyl substituents) of the EuIII complex was selected to prevent crystallization, to inhibit the formation of defects in the structure of films and to provide its uniform distribution in the polymer during polymerization. As a result we obtain an EuIII complex of the film with remarkable thermal behavior the complex melts to isotropic liquid without decomposition, it supercools at ambient temperature and it forms a stable amorphous material at low (up to -30°C) temperatures. The films were prepared by two methods bulk polymerization and spin coating. A comparison of the differences of luminescent and optical characteristics of micro- and nanosized PMMA films doped with the anisometric EuIII complex is given. Based on X-ray powder diffraction and small-angle scattering data, it has been supposed that the association of EuIII complex molecules occurs in the voids of the PMMA matrix and is accompanied by the formation of a nanocrystalline phase. For films obtained by spin coating, a deeper microphase separation is demonstrated than by bulk polymerization. The dimensional characteristics of the nano-associates were determined and a correlation between the method of preparation and the type of distribution of the EuIII complex in the PMMA matrix is established.The atomic structure of nanometre-sized Zn-Zr precipitates in a Mg alloy is determined by combining tilt series of micro-beam electron diffraction with atomic resolution Z-contrast imaging. The stoichiometry of the Zn-Zr precipitates is Zn2Zr3 with a primitive tetragonal structure (space group P42/mnm, a = b = 0.761 nm, c = 0.682 nm). There are 20 atoms in the unit cell of tetragonal Zn2Zr3, comprising 12 Zr atoms at the 4d, 4f, 4g positions and eight Zn atoms at the 8j positions.Diffuse scattering, observed as intensity distribution between the Bragg peaks, is associated with deviations from the average crystal structure, generally referred to as disorder. In many cases crystal defects are seen as unwanted perturbations of the periodic structure and therefore they are often ignored. Yet, when it comes to the structure analysis of nano-volumes, what electron crystallography is designed for, the significance of defects increases. Twinning and polytypic sequences are other perturbations from ideal crystal structure that are also commonly observed in nanocrystals. Here we present an overview of defect types and review some of the most prominent studies published on the analysis of defective nanocrystalline structures by means of three-dimensional electron diffraction.The pair distribution function (PDF) is a versatile tool to describe the structure of disordered and amorphous materials. Electron PDF (ePDF) uses the advantage of strong scattering of electrons, thus allowing small volumes to be probed and providing unique information on structure variations at the nano-scale. The spectrum of ePDF applications is rather broad from ceramic to metallic glasses and mineralogical to organic samples. The quantitative interpretation of ePDF relies on knowledge of how structural and instrumental effects contribute to the experimental data. Here, a broad overview is given on the development of ePDF as a structure analysis method and its applications to diverse materials. Then the physical meaning of the PDF is explained and its use is demonstrated with several examples. Special features of electron scattering regarding the PDF calculations are discussed. A quantitative approach to ePDF data treatment is demonstrated using different refinement software programs for a nanocrystalline anatase sample. Finally, a list of available software packages for ePDF calculation is provided.Multi-slice simulations of electron diffraction by three-dimensional protein crystals have indicated that structure solution would be severely impeded by dynamical diffraction, especially when crystals are more than a few unit cells thick. In practice, however, dynamical diffraction turned out to be less of a problem than anticipated on the basis of these simulations. Here it is shown that two scattering phenomena, which are usually omitted from multi-slice simulations, reduce the dynamical effect solvent scattering reduces the phase differences within the exit beam and inelastic scattering followed by elastic scattering results in diffusion of dynamical scattering out of Bragg peaks. Thus, these independent phenomena provide potential reasons for the apparent discrepancy between theory and practice in protein electron crystallography.Electron diffraction tomography (EDT) data are in many ways similar to X-ray diffraction data. However, they also present certain specifics. One of the most noteworthy is the specific rocking curve observed for EDT data collected using the precession electron diffraction method. This double-peaked curve (dubbed `the camel') may be described with an approximation based on a circular integral of a pseudo-Voigt function and used for intensity extraction by profile fitting. Another specific aspect of electron diffraction data is the high likelihood of errors in the estimation of the crystal orientation, which may arise from the inaccuracies of the goniometer reading, crystal deformations or crystal movement during the data collection. A method for the refinement of crystal orientation for each frame individually is proposed based on the least-squares optimization of simulated diffraction patterns. This method provides typical angular accuracy of the frame orientations of less than 0.05°. These features were implemented in the computer program PETS 2.0. selleck The implementation of the complete data processing workflow in the program PETS and the incorporation of the features specific for electron diffraction data is also described.The diffraction patterns acquired with transmission electron microscopes gather reflections from all crystallites that overlap in the foil thickness. The superimposition renders automated orientation or phase mapping difficult, in particular when secondary phase particles are embedded in a dominant diffracting matrix. Several numerical approaches specifically developed to overcome this issue for 4D scanning precession electron diffraction data sets are described. They consist either in emphasizing the signature of the particles or in subtracting the matrix information out of the collected set of patterns. The different strategies are applied successively to a steel sample containing precipitates that are in Burgers orientation relationship with the matrix and to an aluminium alloy with randomly oriented Mn-rich particles.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.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.Scanning diffraction experiments are approaches that take advantage of many of the recent advances in technology (e.g. computer control, detectors, data storage and analysis) for the transmission electron microscope, allowing the crystal structure of materials to be studied with extremely high precision at local positions across large areas of sample. The ability to map the changing crystal structure makes such experiments a powerful tool for the study of microstructure in all its forms from grains and orientations, to secondary phases and interfaces, strain and defects. This review will introduce some of the fundamental concepts behind the breadth of the technique and showcase some of the recent developments in experiment development and applications to materials.Electron diffraction tomography (EDT) has gained increasing interest, starting with the development of automated electron diffraction tomography (ADT) which enables the collection of three-dimensional electron diffraction data from nano-sized crystals suitable for ab initio structure analysis. A basic description of the ADT method, nowadays recognized as a reliable and established method, as well as its special features and general applicability to different transmission electron microscopes is provided. In addition, the usability of ADT for crystal structure analysis of single nano-sized crystals with and without special crystallographic features, such as twinning, modulations and disorder is demonstrated.A group-theoretical framework to describe vacancy ordering and magnetism in the Fe1-xS system is developed. This framework is used to determine the sequence of crystal structures consistent with the observed magnetic structures of troilite (FeS), and to determine the crystallographic nature of the low-temperature Besnus transition in Fe0.875S. It is concluded that the Besnus transition is a magnetically driven transition characterized by the rotation of the moments out of the crystallographic plane to which they are confined above the transition, accompanied by small atomic displacements that lower the symmetry from monoclinic to triclinic at low temperatures. Based on the phase diagram, magnetically driven phase transitions at low temperatures are predicted in all the commensurate superstructures of pyrrhotite. Based on the phase diagram, magnetically driven spin reorientations at low temperatures are predicted in all the commensurate superstructures of pyrrhotite. The exact nature of the spin rotation is determined by the symmetry of the vacancy-ordered state and based on this spin-flop transitions in 3C and 5C pyrrhotite and a continuous rotation akin to that seen in 4C pyrrhotite are predicted. A Besnus-type transition is also possible in 6C pyrrhotite. Furthermore, it is clarified that 3C and 4C pyrrhotite carry a ferrimagnetic moment whereas 5C and 6C are antiferromagnetic.
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