Микроструктура и фазовый состав сплава дисилицидов железа и хрома

The phase composition, microstructure, and interphase interfaces of the disordered CrSi2-FeSi2 solid solution obtained by spontaneous crystallization (before and after annealing) have been investigated by scanning, transmission electron microscopy, electron diffraction, and X-ray energy dispersive spectrometry. The as-grown samples contained the phases of CrSi2 with the P6422 hexagonal structure and FeSi2 with the P4/mmm tetragonal structure. Annealing of the samples led to the phase transformation of tetragonal FeSi2 into the orthorhombic modification Cmca. Precipitates of cubic iron monosilicide FeSi with space group P213, nano-precipitates of Si and silicon silicide Cr5Si3 with a tetragonal structure I4/mcm were observed inside the FeSi2 grains. Impurities of interstitial Cr atoms with a concentration up to 2.0 at% are found in iron (di)silicides grains in all samples. The structure of the CrSi2 phase remains unchanged after annealing; the concentration of impurity iron atoms is about 0.7 at%. Orientation relationships between the crystal lattices of the phases are established and strains due to the mismatch of the crystal lattices are determined.

Structure of boehmite-derived γ-alumina and its transformation mechanism revealed by electron crystallography

γ-Alumina is a used material, while its precise crystal structure and transformation mechanism derived from boehmite have remained unclear in the literature for decades. In this work, quantitative electron microscopy has been applied to study the crystalline structure of γ-alumina and its transformation mechanism from boehmite. Based on Rietveld refinement of electron diffraction patterns, a new tetragonal structure model, with a space group of I41/amd (No. 141), was proposed for the γ-alumina phase, with Al cations on 4a, 8c, 8d and 16g sites and O anions on the 16h site, which could provide better fits than current models. During the boehmite to γ-alumina transformation induced by e-beam irradiation, when the boehmite layers were oriented along the edge-on direction, a shrinkage caused by dehydration was directly observed. Two kinds of boehmite to γ-alumina transformation mechanisms, namely collapse and reaction mechanisms, were elucidated crystallographically in detail with new insights through an intermediate structure, and the reaction mechanism was demonstrated to produce much reduced changes in dimensions and volume, compared with the collapse mechanism. The experimental observations supported the reaction mechanism, which occurred through partial occupation of the dehydrated space by diffusion in the initial stage of the transformation, without the formation of voids that only appeared after the initial stage. Filling tetrahedral interstices of the intermediate structure with Al cations in different ways yields tetragonal or cubic γ-alumina structures, and the tetragonal structure is energetically favorable because of smaller lattice distortions required, compared with the cubic structure. The crystallographic orientation relationships of γ-alumina with the parent boehmite phase deduced from the proposed mechanisms are consistent with the experimental observations.

Nanostructural crystallization of metals

Based on thermodynamic calculations, it is shown that metal crystallization is an equilibrium nanostructural process. At the beginning, trigonal or tetragonal structure-forming nanocrystals are formed from elementary nanocrystals. Then crystallization centers are formed from them. Further, tetragonal or hexagonal dendrites are formed from them and tetragonal or trigonal structure-forming nanocrystals. Their forms depend on the degree of branching of dendrites. The most branched of them (compact dendrites) are tetragonal or hexagonal crystals.

Effect of a Sulfur Precursor on the Hydrothermal Synthesis of Cu2MnSnS4

Cu2MnSnS4 (CMTS) is acknowledged as an alternative to traditional semiconductors. The structure and microstructure of synthetic CMTS depend on, among other things, the types of sulfur sources used. Traditionally obtained CMTS mostly has a tetragonal structure. In this study, the effect of using thiourea (Tu) or Na2S as a sulfur source on the product structure was compared using hydrothermal synthesis at 190 °C for 7 days (ethylene glycol with water in the presence of poly(vinylpyrollidone) was used as a solvent). When Tu was used, CMTS precipitated in the form of concentric microspheres, 1–1.5 µm in size, consisting of hexagonal (in the cores) and tetragonal (the rims) forms. Most probably, the rapidly formed hexagonal nucleus was later surrounded by a slower-forming rim with a tetragonal structure. In contrast, when Na2S was used as a precursor, microspheres were not formed and a fine crystalline material with a homogeneous tetragonal structure was obtained. This allowed for the choice of micromorphology and product structure during synthesis.

Morphology of Dispersoids in an Annealed Al-Mg Alloys

Morphology of dispersoids in an annealed Al-Mg alloy were investigated using TEM. Five kinds of dispersoids with different structures and morphologies were observed in an annealed Al-Mg alloy. The 1st, or spherical-like one is monoclinic structured θ-Al45(Mn,Cr)7 phase with twin and orientation domain. The 2nd or plate-shaped one is η-Al5(Mn,Cr) phase with monoclinic or pesuo-tetragonal structure. The 3rd or prismatic-like one is a new hexagonal structured Al6.4Mn phase with a unit cell of a=1.72nm, c=1.27nm, and γ=120°, and the 4th or big rod-shaped one is orthorhombic structured Al6(Mn,Fe) phase which is often reported. The 5th one is E-Al18Mg3(Mn–Cr)2 phase with twin or triple twin observed occasionally in Al-Mg annealed alloy. The first two of dispersoids are in majority, followed by the middle two and a small number of the fifth. Formation mechanisms of these particles in Al-Mg alloy are discussed according to phase diagram and possible formation of the twins in the particles are described based on minimum energy.

Synthesis, characterization, and photocatalytic efficiency of a new smart PdO oxide nanomaterials for using in the recycling and sustainable wastewater treatment

Nanostructured PdO materials with promising catalytic properties were successfully synthesized by the controlled thermal decomposition in air of three Pd(II) complexes containing Pd(II) ion, ofloxacin drug and amino acid. The Pd(II) complexes which were used as precursors were [Pd(OFL)(Gly)]Cl, [Pd(OFL)(Ala)]Cl, and [Pd(OFL)2]Cl2, where Gly is glycine amino acid, Ala is alanine amino acid, and OFL is ofloxacin. Structural and morphological properties of the synthesized PdO materials were obtained using FTIR, XRD, SEM, and EDX techniques. The XRD results confirm the tetragonal structure of PdO. The obtained PdO materials were tested as a catalyst for the heterogeneous degradation of H2O2 solution. The results revealed that PdO could effectively degrade H2O2. KEY WORDS: PdO, Nanoparticles, Photocatalytic efficiency, Wastewater treatment Bull. Chem. Soc. Ethiop. 2021, 35(1), 107-118. DOI: https://dx.doi.org/10.4314/bcse.v35i1.9