Combined magnetic and structural characterization of hidrothermal bismuth ferrite (BiFeO3) nanoparticles

Bismuth ferrite (BiFeO3) was synthesized by hydrothermal method. The crystal and magnetic structures of BiFeO3 have been studied by means of X-ray diffraction and neutron powder diffraction at ambient temperature. Microstructure was analysed by scanning electron microscopy. Quantitative phase analysis by the Rietveld method was conducted and crystallite sizes of 27 nm were determined from the XRD line broadening. The magnetic structure of BiFeO3 is described by the G-type antiferromagnetic order with magnetic peak located at 4.6 Å and a noticeable magnetic contribution to a reflection located at 2.4 Å in the diffraction pattern. The values of the ordered magnetic moment of Fe ions μFe=3.8(1) μB, obtained at ambient conditions, are consistent with those determined earlier. The magnetic moments in the crystal plane z = const are arranged in parallel, changing the direction from [100] to [ 110 ] when moving from one to the other z = const plane. © 2018 Authors. Published by the International Institute for the Science of Sintering

The DN-6 Neutron Diffractometer for High-Pressure Research at Half a Megabar Scale

A neutron diffractometer DN-6 at the IBR-2 high-flux reactor is used for the studies of crystal and magnetic structure of powder materials under high pressure in a wide temperature range. The high neutron flux on the sample due to a parabolic focusing section of a neutron guide and wide solid angle of the detector system enables neutron diffraction experiments with extraordinarily small volumes (about 0.01 mm3) of studied samples. The diffractometer is equipped with high-pressure cells with sapphire and diamond anvils, which allow pressures of up to 50 GPa to be reached. The technical design, main parameters and current capabilities of the diffractometer are described. A brief overview of recently obtained results is given

A Study of PbF₂ Nanoparticles Crystallization Mechanism in Mixed Oxyde-Fluoride Glasses

Samples of nanocrystalline PbF2 glass ceramics were obtained by heat-treating SiO2–GeO2–PbO–PbF2–CdF2 glasses. The Ho2O3 and Tm2O3 doping effects on the structural features of PbF2 nanoparticles were studied using small-angle X-ray scattering and X-ray diffraction methods. The enlargements of the average sizes of nanoparticles and the sizes of local areas of density fluctuations have been found to be correlated with an increase in concentrations of Ho2O3 and Tm2O3 in initial glasses. A variation in the concentrations of Ho2O3 and Tm2O3 does not affect the morphology and fractal dimension of the formed PbF2 nanoparticles

Structural, Magnetic and Vibrational Properties of Van Der Waals Ferromagnet CrBr3 at High Pressure

The crystal and magnetic structures of van der Waals layered ferromagnet CrBr3 were studied using X-ray powder diffraction and neutron powder diffraction at pressures up to 23 GPa at ambient temperature and up to 2.8 GPa in the temperature range 6–300 K, respectively. The vibration spectra of CrBr3 were studied using Raman spectroscopy at pressures up to 23 GPa at ambient temperature. The anomalous pressure behavior of structural parameters and vibrational modes was observed, associated with a gradual isostructural phase transition in the pressure range 2.5–7 GPa. The Curie temperature TC reduced rapidly with a pressure coefficient dTC/dP=−4.1(4) K/GPa. A full suppression of the ferromagnetic state was expected at PC~8.4 GPa, where onset of the antiferromagnetic spin arrangement or magnetically disordered state may take place. Anomalies in Raman spectra at P~15 GPa point to another possible phase transformation in CrBr3, which may be related to the proximity of metallization of this van der Waals ferromagnet

Pore Segmentation Techniques for Low-Resolution Data: Application to the Neutron Tomography Data of Cement Materials

The development of neutron imaging facilities provides a growing range of applications in different research fields. The significance of the obtained structural information, among others, depends on the reliability of phase segmentation. We focused on the problem of pore segmentation in low-resolution images and tomography data, taking into consideration possible image corruption in the neutron tomography experiment. Two pore segmentation techniques are proposed. They are the binarization of the enhanced contrast data using the global threshold, and the segmentation using the modified watershed technique—local threshold by watershed. The proposed techniques were compared with a conventional marker-based watershed on the test images simulating low-quality tomography data and on the neutron tomography data of the samples of magnesium potassium phosphate cement (MKP). The obtained results demonstrate the advantages of the proposed techniques over the conventional watershed-based approach

Phase Composition and Its Spatial Distribution in Antique Copper Coins: Neutron Tomography and Diffraction Studies

The chemical and elementary composition, internal arrangement, and spatial distribution of the components of ancient Greek copper coins were studied using XRF analysis, neutron diffraction and neutron tomography methods. The studied coins are interesting from a historical and cultural point of view, as they are “Charon’s obol’s”. These coins were discovered at the location of an ancient Greek settlement during archaeological excavations on the “Volna-1” necropolis in Krasnodar Region, Russian Federation. It was determined that the coins are mainly made of a bronze alloy, a tin content that falls in the range of 1.1(2)–7.9(3) wt.%. All coins are highly degraded; corrosion and patina areas occupy volumes from ~27 % to ~62 % of the original coin volumes. The neutron tomography method not only provided 3D data of the spatial distribution of the bronze alloy and the patina with corrosion contamination inside coin volumes, but also restored the minting pattern of several studied coins. Taking into account the obtained results, the origin and use of these coins in the light of historical and economic processes of the Bosporan Kingdom are discussed

Studies of Ancient Russian Cultural Objects Using the Neutron Tomography Method

Neutron radiography and tomography is a non-destructive method that provides detailed information about the internal structure of cultural heritage objects. The differences in the neutron attenuation coefficients of constituent elements of the studied objects, as well as the application of modern mathematical algorithms to carry out three-dimensional imaging data analysis, allow one to obtain unique information about the spatial distribution of different phases, the presence of internal defects, or the degree of structural degradation inside valuable cultural objects. The results of the neutron studies of several archaeological objects related to different epochs of the Russian history are reported in order to demonstrate the opportunities provided by the neutron tomography method. The obtained 3D structural volume data, as well as the results of the corresponding data analysis, are presented

Structural and magnetic properties of Cr2O3\mathrm{Cr_{2}O_{3}} at high pressure

The structural and magnetic properties of Cr$_{2}$O$_{3}$ have been studied by means of X-ray and neutron powder diffraction at high pressures up to 35 GPa. The lattice compression of the rhombohedral crystal structure of R $\bar{3}$c symmetry is slightly anisotropic with anomaly in the pressure behavior of the c/a parameters ratio at P $\approx$ 20 GPa of presumably magnetic nature. The oxygen octahedra around chromium ions become more symmetric with close values of shared and unshared bonds under high pressure. The antiferromagnetic structure of Cr$_{2}$O$_{3}$ remains stable in the studied pressure range up to 35 GPa. The pressure coefficient of the Neel temperature, (1/T$_N$)(dT$_N$/dP) = + 0.0091 GPa$^1$, is significantly less in comparison with perovskite-like compounds containing Cr$^{3+}$ and Mn$^{4+}$ ions of similar electronic configuration

Spin-induced multiferroicity in the binary perovskite manganite Mn2O3

The ABO3 perovskite oxides exhibit a wide range of interesting physical phenomena remaining in the focus of extensive scientific investigations and various industrial applications. In order to form a perovskite structure, the cations occupying the A and B positions in the lattice, as a rule, should be different. Nevertheless, the unique binary perovskite manganite Mn2O3 containing the same element in both A and B positions can be synthesized under high-pressure high-temperature conditions. Here, we show that this material exhibits magnetically driven ferroelectricity and a pronounced magnetoelectric effect at low temperatures. Neutron powder diffraction revealed two intricate antiferromagnetic structures below 100 K, driven by a strong interplay between spin, charge, and orbital degrees of freedom. The peculiar multiferroicity in the Mn2O3 perovskite is ascribed to a combined effect involving several mechanisms. Our work demonstrates the potential of binary perovskite oxides for creating materials with highly promising electric and magnetic properties

The Polymorphic Phase Transformations in the Chlorpropamide under Pressure

The crystal structure and vibrational spectra of the chlorpropamide have been studied by means of the X-ray diffraction andRaman spectroscopy at pressures up to 24.6 and 4.4 GPa, respectively. Two polymorphic phase transitions, between initial orthorhombicform-A and a monoclinic form-AI at P ∼ 1.2 GPa and, in additional, to another monoclinic form-AII at P ∼ 3.0 GPa, were observed.At pressures above 9.6 GPa, a transformation to the amorphous phase of chlorpropamide was revealed. The lattice parameters, unit cellvolumes, and vibration modes as functions of pressure were obtained for the different polymorphic modifications of chlorpropamide