Synthesis of Zinc Ferrites in RF Thermal Plasma Reactor

Formation of nanosized zinc ferrite spinels was studied from iron- and zinc oxide powders and corresponding nitrate solutions, respectively in a radiofrequency thermal plasma reactor. From the viewpoint of applications, the research was motivated by the potential use of these materials in advanced magnetic devices on the one hand, and by their biomedical applications such as drug carriers or agents for cancer treatment by hyperthermia on the other. In this work effects of synthesis conditions on properties of products were studied in details. The products were characterised for chemical composition, phase conditions, particle size distribution, morphologies and saturation magnetisation. Most products exhibited ferrimagnetic behaviour. Correlations among domain- and particle sizes were also investigated. Conditions for the synthesis of nanosized, inverse zinc ferrites of high saturation magnetisation were established. It was proved that in thermal plasma conditions normal and inverse ferrites could be produced in a single step process

Synthesis of Spinel Ferrites in Radiofrequency Thermal Plasma Reactor

Formation of nanosized zinc-ferrites and nickel-zinc ferrites from iron- and zinc oxide powders and corresponding nitrate solutions, respectively, was studied in RF thermal plasma conditions. The products were characterized for chemical composition, phase conditions, particle size distribution, morphologies and saturation magnetization. Effects of synthesis conditions on properties of products were studied in details

Thermal stability of the microstructure of severely deformed copper

Copper specimens were deformed by equal channel angular pressing (ECAP) up to 8 passes. The microstructure was studied by X-ray line profile analysis. The crystallite size is reduced to a few tens of nanometers even after the first ECAP pass and it does not change significantly during further deformation. At the same time, the dislocation density increases gradually up to 4 ECAP passes. The thermal stability of the microstructure is examined by differential scanning calorimetry (DSC). The temperature of the DSC peak decreases whereas the stored energy increases with increasing strain. At the beginning of the heat release a bimodal grain structure develops indicated by a special double-peak shape of the diffraction line profiles

Nanocrystalline materials studied by powder diffraction line profile analysis

X-ray powder diffraction is a powerful tool for characterising the microstructure of crystalline materials in terms of size and strain. It is widely applied for nanocrystalline materials, especially since other methods, in particular electron microscopy is, on the one hand tedious and time consuming, on the other hand, due to the often metastable states of nanomaterials it might change their microstructures. It is attempted to overview the applications of microstructure characterization by powder diffraction on nanocrystalline metals, alloys, ceramics and carbon base materials. Whenever opportunity is given, the data provided by the X-ray method are compared and discussed together with results of electron microscopy. Since the topic is vast we do not try to cover the entire field

Influence of sintering temperature and pressure on crystallite size and lattice defect structure in nanocrystalline SiC

Microstructure of sintered nanocrystalline SiC is studied by x-ray line profile analysis and transmission electron microscopy. The lattice defect structure and the crystallite size are determined as a function of pressure between 2 and 5.5 GPa for different sintering temperatures in the range from 1400 to 1800 degrees C. At a constant sintering temperature, the increase of pressure promotes crystallite growth. At 1800 degrees C when the pressure reaches 8 GPa, the increase of the crystallite size is impeded. The grain growth during sintering is accompanied by a decrease in the population of planar faults and an increase in the density of dislocations. A critical crystallite size above which dislocations are more abundant than planar defects is suggested

Mechanochemical Reactions of Lithium Niobate Induced by High-Energy Ball-Milling

Lithium niobate (LiNbO3, LN) nanocrystals were prepared by ball-milling of the crucible residue of a Czochralski grown congruent single crystal, using a Spex 8000 Mixer Mill with different types of vials (stainless steel, alumina, tungsten carbide) and various milling parameters. Dynamic light scattering and powder X-ray diffraction were used to determine the achieved particle and grain sizes, respectively. Possible contamination from the vials was checked by energy-dispersive X-ray spectroscopy measurements. Milling resulted in sample darkening due to mechanochemical reduction of Nb (V) via polaron and bipolaron formation, oxygen release and Li2O segregation, while subsequent oxidizing heat-treatments recovered the white color with the evaporation of Li2O and crystallization of a LiNb3O8 phase instead. The phase transformations occurring during both the grinding and the post-grinding heat treatments were studied by Raman spectroscopy, X-ray diffraction and optical reflection measurement, while the Li2O content of the as-ground samples was quantitatively measured by coulometric titration

Phase transition in nanomagnetite

Recently, the application of nanosized magnetite particles became an area of growing interest for their potential practical applications. Nanosized magnetite samples of 36 and 9 nm sizes were synthesized. Special care was taken on the right stoichiometry of the magnetite particles. Mössbauer spectroscopy measurements were made in 4.2–300 K temperature range. The temperature dependence of the intensities of the spectral components indicated size dependent transition taking place in a broad temperature range. For nanosized samples, the hyperfine interaction values and their relative intensities changed above the Verwey transition temperature value of bulk megnetite. The continuous transition indicated the formation of dendritelike granular assemblies formed during the preparation of the samples

Characterization of defect structures in nanocrystalline materials by X-ray line profile analysis

X-ray line profile analysis is a powerful alternative tool for determining dislocation densities, dislocation type, crystallite and subgrain size and size-distributions, and planar defects, especially the frequency of twin boundaries and stacking faults. The method is especially useful in the case of submicron grain size or nanocrystalline materials, where X-ray line broadening is a well pronounced effect, and the observation of defects with very large density is often not easy by transmission electron microscopy. The fundamentals of X-ray line broadening are summarized in terms of the different qualitative breadth methods, and the more sophisticated and more quantitative whole pattern fitting procedures. The efficiency and practical use of X-ray line profile analysis is shown by discussing its applications to metallic, ceramic, diamond-like and polymer nanomaterials

Microstructure of nanocrystalline diamond powders studied by powder diffractometry

High resolution x-ray diffraction peaks of diamond nanosize powders of nominal sizes ranging from 5 to 250 nm were analyzed and provided information on grain structure, average size of crystallites, and concentration of dislocations. Selected samples were heat treated at 1670 K at pressures 2.0 and 5.5 GPa or had surface modified by outgassing, heat treatment at vacuum conditions, and by controlled adsorption of gases. The apparent lattice parameter method was applied to characterize the structure of a shell-core model of nanosize particles. The multiple whole profile fitting provided information on crystallite sizes and density of dislocations. Population of dislocations increased with applied pressure, while strain and interplanar distances in the surface layers decreased. Adsorption of foreign gases on the grain surface modified the structure of the surface layers but did not affect dislocations near the center of the grains