Solid State Phenomena Vol. 186

Abstract: The electron tomography and transmission electron microscopy studies of the carbides in the 0.5Cr-0.5Mo-0.25V (13HMF) low-alloy steel after service during 160 000 h at 540 °C were carried out. Identification of the carbides was performed by means of electron diffraction analysis. Meso-scale tomography technique, mainly FIB/SEM tomography, was used for detailed characterization of spatial distribution and metrology of the carbides in 13HMF steel. The results achieved confirm the ability of FIB tomography to get 3D reconstruction of internal microstructure of steel as well as to obtain information about the shape and spatial distribution of carbides.

Abstract: In the present work a quantitative analysis of γ' and γ" phase nanoparticles in Inconel 718 was performed using two methods of electron tomography, namely EFTEM and FIB tomography. 3D visualisation showed that γ' particles are spherical, while γ" precipitates are disc-shaped. The values of mean size of γ' and γ" phase particles, determined by both electron tomography methods applied, are in good agreement.

Abstract: Presented work summarizes studies done on the course of the martensitic transformation in the Ti50Ni25Cu25 alloy. Studies were carried out using scanning electron microscopy JEM 6480 equipped with an electron back scattered detector (EBSD) as well as a heating attachment. As-received ribbon was mainly amorphous. At the free side of the ribbon some fine randomly oriented crystalline grains were formed. During heating followed by cooling the reversible martensitic transformation occurred with sequence: B2↔B19. The crystallographic correlation between the B2 phase and the B19 martensite were confirmed. It allowed finding transformation matrix between both phases.

Abstract: New subdivision of microscopic investigation called Orientation Microscopy (OM) is already well known in scanning electron microscope (SEM). Needs for investigation in nanoscale contribute to development of an appropriate method for transmission electron microscope (TEM). Automated acquisition and indexing of diffraction patterns, necessary for creation of orientation maps in TEM, cause more difficulties then in SEM. Nevertheless, the techniques of OM are also being developed in the Transmission Electron Microscope (TEM). Microdiffraction has been successfully introduced for creating such maps. Individual orientation measurements, which appeared in the convergent beam mode, can be used for quantitative description of microstructure of fine grained and deformed materials. The idea of the operation of the automated system in transmission electron microscope (TEM) which is developed in IMIM PAS relies on an automatic (with control position of the beam) acquisition of diffraction patterns using digital CCD camera, and indexing them, and then on the analysis of the set of individual crystallographic orientations. The graphic presentation of received sets of orientation can be analysed in order to obtain parameters and characteristics such as texture characteristics, characteristics of grain boundaries (based on orientation relationship) or the stereological characteristics. To illustrate application of this system, orientation maps measured in cold-rolled polycrystalline aluminium and its alloy 6013, and in multi-phase alloys of Fe-Cr-Co system after severe plastic deformation are presented.

Abstract: Aero engine turbine blades made of nickel-based superalloys are critical components in flight safety. Therefore, it is very important to make sure that the chemical composition, phase composition and microstructure are suitable. However, due to their chemical compositions, superalloys are prone to many transformations and the formation of deleterious phases, which deteriorate the mechanical properties. Hence, investigations concerning the structural stability and phase identification—especially topologically close-packed phases (TCP)—are necessary. Because the volume fractions of these phases are generally small, phase identification should be performed by nanodiffraction techniques in a scanning transmission electron microscope (STEM) and electron backscatter diffraction in a scanning electron microscope (EBSD/SEM). These methods complement each other, but each of them is characterized by different difficulties and limitations. In this paper we present the possibilities and limitations of phase identification in single crystal CMSX-4 superalloy after long thermal exposure.

Abstract: Modern scanning electron microscopes (SEMs) increase the ability to study a wide range of materials. Especially, an application of low vacuum conditions enables characterization of nonconductive samples without complicated preparation procedure. However, the operator must be aware of several problems he may encounter collecting electron diffractions in the SEM with variable pressure. The charge control and quality of the surface are the challenges when running experiments on insulators. Specimen charging obscures forward scatter electrons images and decreases the EBSD pattern quality making indexing difficult or even impossible. Another crucial question is how to limit the influence of so called "skirt effect" caused by ionization of gas molecules followed by electron beam broading above the sample. The influence of several important parameters (gas pressure, a type of gas, working distance and energy of electron beam) on the EBSD pattern quality must also be considered. When it is properly done, a coupling of crystallographic information with the chemical data obtained from Energy Dispersive Spectroscopy (EDS) in the LV-SEM allows to perform phase identification of insulators. The paper presents some ideas how to deal with the (Pb, La)(Zr, Ti)O₃ ceramics in high resolution Quanta 3D SEM (with thermally assisted Schottky type FEG) equipped with EDAX-TSL system in low vacuum environment. The problems occurring during EBSD analysis of the PLZT ceramics are discussed and some solutions are suggested. Paper summarizes the results obtained from PLZT ferroelectric ceramics in the low vacuum FEGSEM and shows how to optimise experimental parameters in order to achieve the best quality of orientation maps acquired from nonconductive samples.

Abstract: We present results of the study on the silicon nanoparticles formation in multilayer silicon nitride structures. These structures consist of pairs of stoichiometric silicon nitride dielectric layers (SiN_x) and silicon rich nitride layers (SRN). Silicon nanocrystals precipitate from the SRN layer during annealing at high temperatures (1000 °C or 1100 °C). High resolution transmission electron microscopy has been applied for investigation of the nanocrystals formation. Surface photovoltage spectroscopy technique was used for the spectral characterization of prepared structures

Abstract: Growth of high quality GaN/AlN heterostructures by plasma assisted molecular beam epitaxy (PAMBE) is possible with excess of Ga on the surface. During growth of AlN this additional Ga acts as surfactant and improves mobility of the Al adatoms on the growing surface, at the possible cost of Ga segregation and creation of mixed AlGaN interlayer. Scanning transmission electron microscopy (STEM) and electron energy loss spectroscopy (EELS) were used to determine chemical composition of high crystallographic quality GaN-AlN multilayer structure. It was shown that segregation occurs at AlN-GaN heterointerfaces, while GaN-AlN interfaces have abrupt stepwise change of the chemical composition. HRTEM results show creation of trench defects at the periphery of growing AlN islands in the case of nonoptimized growth.

Abstract: This paper describes Transmission Electron Microscopy studies of the structural changes of GaN1-xAsx alloys grown by Molecular Beam Epitaxy at low temperatures on Al2O3 substrate. We found that by lowering the growth temperature increasing amount of As can be incorporated in GaN1-xAsx forming a single phase alloy. For the low As content a columnar growth of wurtzite structure is observed but for increasing As in the range of 0.170.75 the layer becomes amorphous. Increase in Ga flux at low growth temperature (about 200°C) leads to columnar alloys with As content >75% with a cubic structure. In addition to the structural changes monotonic change of the band gap is also observed with the As content in the alloy. The amorphous alloy is stable up to annealing at temperatures not higher than 600°C. Annealing at higher temperature leads to phase separation of GaAs:N and GaN:As confirmed by Z-contrast electron microscopy.

Abstract: Transmission electron microscopy (TEM) techniques were used for characterization of annealing (400, 600 and 800 °C) influence on the structural properties of the HfO₂ film (45 nm thick) deposited on Si substrate. Such structures are considered as high-k dielectric materials for application in novel semiconductor devices. The studies showed that independently of the annealing temperature a very thin and flat amorphous layer is formed between HfO₂ layer and Si substrate. This result was also found in the non-annealed sample. EDXS examination confirmed that the stoichiometry for the hafnium oxide layer in each sample corresponds to 1:2 for Hf:O (i.e. to HfO₂). TEM images revealed differences in the microstructure of HfO₂ layers in annealed samples, however the layers have similar thickness and interface roughness in all studied samples.