Papers by Keyword: Electron Microscopy

Abstract: Commercially pure aluminium powder and a mixture of aluminium and silicon powders, both in a liquid amyl acetate-based organic binder, were sprayed onto the surface of Inconel 713LC nickel base superalloy. A two-stage heat treatment process in an argon atmosphere flow was designed and applied to produce nickel aluminide diffusion coatings. Two coating systems composed of different layers with gradual changes in chemical composition and phase quantities were formed. Scanning electron microscope, scanning electron microscope/focused ion beam, both equipped with energy dispersive microanalyzers, were utilized to characterize the microstructure and chemical composition of the coatings.

Abstract: Susceptibility to cracking of the as-cast C-Mn-Cr-Nb steel was studied by laboratory rolling. The variable parameters were the heating temperature (1150 - 1340 °C) as well as the rolling temperature (950 - 1150 °C). Final microstructure of the free-cooled samples was constituted by bainite, pearlite and ferrite with different morphology and various contribution. Deformation temperature below 1000 °C yielded in the incomplete recrystallization of austenite. Surface cracks originated preferentially on the austenite grains boundaries. Size of the present particles (inclusions and precipitates) varied from 10¹ nm to 10¹ μm. SEM and EDS analysis revealed that the inclusions ware mostly of the MnS type. TEM analysis confirmed that the grain boundaries were not enriched by any particles. In addition to the Fe₃C particles, the discoid niobium carbide particles with approximately 40 nm diameter and 10 nm thickness were detected. These small particles were not connected by any notable pinning of dislocations.

Abstract: The aim of the experiments was to study the influence of the rolling reduction in thickness on the size and distribution of secondary particles and recrystallization behaviour of Al-Mn sheets with Zr addition prepared by twin-roll casting (TRC) in the industrial conditions. Samples, cold rolled on a laboratory mill, were subjected to a one and two-step precipitation annealing. Their microstructure (grain structure, phase composition, particle analysis) and mechanical and physical properties (microhardness, electrical conductivity) were then characterized. Quantitative particle analysis was carried out on field-emission gun scanning electron microscope (FEG-SEM) micrographs.

Abstract: The structure and magnetic properties of multi-walled carbon nanotubes produced by catalytic pyrolysis of methane have been investigated by means of mutually complementary physical methods. The average sizes and number of carbon layers forming nanotubes, smearing of the density of states near the Fermi level, degeneracy temperature of gas of extrinsic current carriers, concentrations of localized spins and extrinsic two-dimensional current carriers have been determined. The conclusion has been drawn that ferromagnetic nanoparticles are present in the inner regions of nanotubes, including their tubular cavities. The difference in electronic structure near the Fermi level for carbon nanotubes and ordered graphite has been revealed. The possible reason is that the electronic states near zigzag-type sites of ends as well as edges of linear structural defects in nanotubes make greater contribution to the spectrum than that from similar sites of graphite.

Abstract: The paper presents experimental results showing the nature of the destruction in the surface layer of В₄С ceramics during hardness and fracture toughness tests performed by Vickers diamond pyramid indentation with different applied loads (4.91 - 294.3 N). Ceramics made from boron carbide powder with 10 wt.% additive of submicron fraction of the same powder sintered in spark discharge plasma by Spark Plasma Sintering (SPS-method) under different sintering conditions was studied. Changes of micro hardness and hardness of the samples were measured by micro hardness tester PМТ-3М with the loads Р up to 4.9 N; by micro hardness tester Micromet with P= 9.811.77 N; and by hardness tester ТP-7R-1 with the loads of 49 - 294.3 N. Indentation, exposure, and unloading were carried out according to standard method during 30-40 seconds. The microstructure and topography of the surface of ceramic samples splits after indentation were studied by scanning electron microscopy (SEM, microscope JEOL SEM-7500FA). The profiles of the split surface depth were determined by Linnik interferometer МII-4.

Abstract: The effect of calcination temperature for Fe₂O₃/MgO catalysts on the formation of carbon nanotubes (CNTs) was examined. CNTs were synthesized over Fe₂O₃/MgO catalysts calcined at different temperatures by catalytic decomposition of methane at 1000°C. The synthesized CNTs were investigated by a combination of scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectroscopy. The results show that the effect of calcination temperatures greatly governed the diameter and the quality of the SWCNTs formed. The catalysts calcined at 500, 600 and 700°C produced CNTswith the diameters of 1.53, 1.95 and 2.97nm, respectively. Generally, an increase in the calcination temperature increases the average diameter and decreases the quality of the CNTs produced.

Abstract: This paper presents the results of analysis of superalloys microstructures with different structures: polycrystalline nickel-based superalloy René 80, Mar-M 200Hf directionally solidified with columnar grains and single crystal CMSX-4. Microstructure studies were performed using a scanning electron microscope Hitachi FE-SEM SU-70 and S-3400N equipped with a Thermo Scientific Noran System for analysis of chemical composition by X-ray dispersion. Metallographic microsections of the rods before and after heat treatment was performed, which were electrolytically etched using different reagents. The morphology of γ phase precipitates in the interdendritic areas and dendritic cores was analyzed. Single crystal rods of nickel superalloy CMSX-4 were cast by Bridgman technique in a vacuum furnace of ALD Vacuum Technologies. Rods were withdrawn with rate: 1mm/min and 5mm/min. EDS X-ray microanalysis showed significant differences in chemical composition between the cores dendrites and eutectic regions. Significant differences in the number of dendrites, the shape and length of the arms were observed. A lower speed rate causes that amount of eutectic is lower but value of primary dendrite arm spacing is higher, while a higher withdraw rate increases the amount of eutectic and decreases primary dendrite arm spacing.

Abstract: Cobalt-boron nanoparticles have been synthesized by a chemical reaction between NaBH₄ and CoCl₂.₆H₂O through manipulating pH value of the reaction mixture. The morphology, structure, phase composition, and thermal behavior have been examined via FESEM, TEM, XRD, EDS, and DSC techniques, respectively. It is demonstrated that the morphology and structure of ultimate nanoparticles completely depends on the pH value of reaction mixture. While the neutral pH value favors the smallest nanoparticles with a mean particle size of 50 nm and complete amorphous structure, the acidic condition promotes the growth process and the crystal structure. Furthermore, these nanoparticles transform into cobalt nanocrystallites after heated at 600°C, and retained the discrepancies in the morphology and the structure of the parent cobalt-boron nanoparticles. A detailed characterization of the nanoparticulates, discussions on the synthesis mechanism, and subsequent formation transformation have been provided.

Abstract: Microstructure of Cu-2wt.%Co alloy after various heat treatment (and hence with various phase constitution) was studied after equal-channel angular pressing (ECAP) using transmission electron microscopy (TEM) and electron backscatter diffraction (EBSD) technique in a scanning electron microscope (SEM). We also focused on local mechanical properties measured across the section perpendicular to the ECAP extrusion direction. Starting from the grain size well above 1mm in the Cu-2wt.%Co solid solution, ECAP subsequently reduces grain size down to the submicron level. A comparison with pure Cu shows that the grain size homogenization is shifted towards higher number of ECAP passes. Fine dispersion of precipitates further slows down the grain refinement and grain size homogenization during ECAP processing. Local mechanical properties measured across the section perpendicular to the ECAP extrusion direction reveal systematic inhomogeneities of deformed microstructure caused by local gradients of temperature and pressure and by the processing geometry itself. This should be considered while characterizing the microstructure by a single EBSD measurement on a small selected area.

Abstract: The effect of irradiation with heavy ions Ne, Ar, and Kr of various energies on the structure and properties of ceramic barium cerate doped with neodymium and annealed in air at 650°C for 7 hours is studied. It is noted that blistering was observed on cerate surface during its irradiation by low energy Ne ions, whereas it was not observed under low-energy Ar and Kr ions irradiation. Irradiation of the cerate with high energy ions caused partial amorphization of the irradiated surface of the material, while the structure of the non-irradiated surface did not change. In addition, the irradiated surface of the cerate endured solid-phase structural changes. Thus, upon high-energy ions irradiation in the range of Ne, Ar, Kr the cerate surface resembled the stages of spherulite formation - nucleation, growth (view of cauliflower), formation of spherulitic crust, respectively. The increase in water molecules release and reduction of molecular oxygen release from the barium cerate, irradiated by high-energy ions is found during vacuum constant rate heating. It is concluded that cerates undergo changes to the distances significantly exceeding the ion ranges in these materials. Features of high-energy ions influence on thermal desorption of carbon dioxide from cerates show, apparently, the formation of weakly bound carbonate compounds on the cerate surface in the irradiation process.