Papers by Author: Jakub Čížek

Abstract: Microstructure of ultra fine grained (UFG) Mg-Gd alloy prepared by high-pressure torsion (HPT) was investigated in the present work. Lattice defects introduced by HPT were characterized at first. Subsequently thermal stability of UFG structure and its development with annealing temperature were studied and correlated with changes of hardness and ductility. Precipitation effects in the alloy with UFG structure were compared with those in a conventional coarse-grained alloy. Defect studies were performed by positron annihilation spectroscopy (PAS), which represents well established non-destructive technique with a high sensitivity to open volume lattice defects like vacancies, dislocations, misfit defects etc. PAS investigations were combined with transmission electron microscopy (TEM) and X-ray diffraction (XRD). Changes of mechanical properties were monitored by Vicker’s microhardness (HV) and deformation tensile tests. It was found that HPT deformed Mg-Gd alloy exhibits UFG structure with mean grain size of 100 nm and a dense network of dislocations distributed uniformly throughout the whole sample. Although recovery of dislocations takes place at relatively low temperatures, it is not accompanied by grain growth and the mean grain size remains around 100 nm up to 300oC. Tensile tests performed at elevated temperatures to examine ductility showed that HPT-deformed alloy exhibits a superplastic behavior at 400oC. Moreover, it was found that the precipitation sequence in HPT-deformed alloy differs from that in conventional coarse-grained material.

Abstract: In this contribution we report on the theoretical study of basic vacancy-like defects in cubic zirconia and yttria stabilized zirconia. In particular, we concentrate on oxygen vacancy, zirconium vacancy and oxygen vacancy – yttrium complex. Relaxed atomic configurations of studied defects are obtained by means of an ab initio pseudopotential method within the supercell approach. Positron characteristics, like positron lifetime and binding energy to defects, are calculated using self-consistent electron densities and potentials taken from ab initio calculations.

Abstract: Hydrogen is an important impurity in zinc oxide and can be incorporated into the lattice in several ways. Hydrogen can be also bound by vacancies that can be studied using positron annihilation techniques. Here we examine theoretically oxygen and zinc vacancies in ZnO, the latter also with hydrogen atoms inside. Several computational approaches are employed to determine the defect geometries and related positron characteristics. Positron-induced forces are also taken into account. Calculated positron lifetimes are compared with those observed in experiment, which gives an indication of the presence of zinc vacancy-hydrogen complexes in ZnO materials.

Abstract: Mg-Tb-Nd ternary alloy represents a novel hardenable Mg-based alloy with enhanced strength and favorable creep properties. In the present work we studied microstructure of ultra fine grained (UFG) Mg-Tb-Nd alloy prepared by high pressure torsion (HPT). Lattice defects introduced into the specimen by the severe plastic deformation play a key role in physical properties of UFG specimens. It is known that positron lifetime (PL) spectroscopy is highly sensitive to open volume defects (like vacancies, dislocations, etc.). Therefore, PL spectroscopy is an ideal tool for defect characterizations in the HPT deformed specimens. In the present work we combined PL studies with transmission electron microscopy and microhardness measurements. After detailed characterization of the as-deformed structure, the specimens were step-by-step isochronally annealed and we investigated the development of microstructure with increasing temperature.

Abstract: Technical purity Cu (99.95 wt%) polycrystals have been processed at room temperature by equal channel angular pressing. The results of mechanical tests and the microstructure characterization by various experimental techniques are presented. The yield stress as well as the strength were shown to increase with increasing strain and exceed the respective values of a coarsegrained material. The microstructure development and its fragmentation after ECAP was investigated by the TEM and EBSD. The proportion of high angle grain boundaries was found to increase with increasing strain reaching the value of 90% after 8 ECAP passes. Two kinds of defects were identified in ECAP specimens by positron annihilation spectrometry (PAS): (a) dislocations which represent the dominant kind of defects, and (b) small vacancy clusters (so called microvoids). The main increase of defect density was found to occur during the first ECAP pass. PAS analysis indicated that in the specimens subjected to one ECAP pass the mean dislocation density ρD and the concentration of microvoids cν exceeded the values of 1014 m-2 and 10-4 at.-1, respectively. After 4 passes, the number of defects becomes saturated and practically does not change with increasing strain.

Abstract: Defect studies of neutron-irradiated Cr-Mo-V (VVER-440) type reactor pressure vessel steels were performed in the present work. The steels were irradiated in the nuclear power plant reactor under the conditions of a regular operation. Characterization of the irradiation induced defects was performed by two complementary techniques of positron annihilation spectroscopy: (i) positron lifetime spectroscopy was used for identification of defects and determination of defect densities, (ii) coincidence Doppler broadening was employed for investigation of Cu atom aggregates. Long range diffusion of Cu atoms is assisted by the irradiation induced vacancies. The solute Cu atoms form small clusters in the irradiated steels. Subsequent isochronal annealing of the irradiated steel leads to vacancy assisted clustering of Cu atoms and formation of small precipitates. The Cu clusters exhibit maximum diameter at 400oC. Above this temperature the clusters dissolve again in the matrix.

Abstract: Precipitation effects in ultra fine grained (UFG) lightweight Mg-based alloys were studied in the present work by means of positron lifetime spectroscopy, transmission electron microscopy, and microhardness. The UFG samples with grain size around 100 nm were fabricated by high pressure torsion (HPT). The UFG structure contains a significant volume fraction of grain boundaries and exhibits a high number of lattice defects (mainly dislocations) introduced by severe plastic deformation during the HPT processing. A high dislocation density and volume fraction of grain boundaries enhance the long range diffusion of solute elements. Moreover, dislocations and grain boundaries act as nucleation centers for precipitates. As a consequence, the precipitation effects are facilitated in the UFG alloys compared to the conventional coarse-grained samples. This phenomenon was examined in this work by comparison of the precipitation sequence in Mg alloys with UFG structure and solution treated coarse-grained alloys.

Abstract: It is known that the severe plastic deformation (SPD) induced by Accumulative Roll Bonding (ARB) results in more important grain refinement as compared to conventional rolling. Since ARB enables production of large amounts of ultra-fine grained (UFG) materials, its adoption into industrial practice is favoured. The paper presents the results of a study of high purity aluminium processed by ARB and cold rolling. Microstructure changes induced by both methods were studied by light and transmission electron microscopy. Dislocation density and arrangement were assessed by positron annihilation spectroscopy. Strength evolution was estimated by hardness measurements. Texture measurements were performed by X-ray diffraction. ARB processing results in over twofold increase in hardness. Hardness increases significantly after two ARB cycles and it raises only a little or decreases during subsequent cycles. The increase in hardness induced by conventional rolling is smaller. Positron lifetime measurements reveal a substantial increase of dislocation density at the first ARB cycle and a moderate increase or even a decrease at further cycles. The high fraction of positrons trapped at grain-boundary dislocations gives evidence for substantial grain refinement confirmed by TEM examinations. Grain size of 1.2 􀁐m in the rolling plane and as small as of 90 nm in the normal direction is obtained. The rolled samples have a typical rolling texture (􀁅-fibre). The 􀁅- fibre of the sample ARB processed to strain of 2.4 is weaker as compared to its rolled counterpart and it presents through thickness variations. The surface layers do not have any 􀁅-fibre orientations but they have ND-rotated cube texture formed by the shear strains induced by lubricant-free rolling.

Abstract: Accumulative Roll Bonding (ARB) does not require any special equipment and enables the production of large amounts of ultra-fine grained (UFG) materials. Grain refinement is thermally stable in materials with finely dispersed particles such as twin-roll cast (TRC) aluminium alloy sheets, favourable materials for manufacturing UFG sheets. The results of a study of the effect of ARB temperature on bonding quality, structure and properties of TRC AA8006 sheet are presented. Examinations by light and transmission electron microscopy, positron annihilation spectroscopy (PAS), hardness and tensile tests were used in the study. After two cycles at 200°C, mean grain size of 0.4 - 0.8 μm is achieved, but areas with extremely fine grains of 0.1 to 0.3 μm in diameter are also observed. Hardness increases significantly after two cycles and it rises a little in subsequent cycles. Processing at higher temperatures (up to 350°C) results in better bonding but it produces smaller increase in hardness. Significant increase of dislocation density is observed by PAS after the first cycle at 250°C but it does not continue during subsequent cycles. Partial recrystallization occurs in samples processed at temperatures above 250°C explaining the smaller increase in hardness. Softening level depends on both ARB temperature and number of cycles. The thermal stability of refined structures produced by ARB at 250°C is better than these formed at higher temperatures.

Abstract: In the present work we studied microstructure of ultra fine grained (UFG) pure Mg and UFG Mg-based alloys. The initial coarse grained samples were deformed by high pressure torsion (HPT) using pressure of 6 GPa. Such deformation leads to formation of UFG structure in the samples. The severe plastic deformation results in creation of high number of lattice defects. Therefore, we used positron annihilation spectroscopy (PAS) for defect characterizations. PAS represents a well developed non-destructive technique with high sensitivity to open volume defects like vacancies, vacancy clusters, dislocations etc. In the present work we combined PAS with TEM and XRD to obtain complete information about microstructure of the UFG samples studied. We have found that microstructure of HPT-deformed Mg contains two kinds of regions: (a) ”deformed” regions with UFG structure (grain size 100-200 nm) and high number of randomly distributed dislocations, and (b) ”recrystallized” regions with low dislocation density and grain size of few microns. It indicates some kind of dynamic recovery of microstructure already during HPT processing. On the other hand, homogenous UFG structure with grain size around 100 nm and high density of homogeneously distributed dislocations was formed in HPT-deformed Mg-9.33 wt.%Gd alloy. After characterization of the as-deformed microstructure the samples were subsequently isochronally annealed and the development of microstructure with increasing temperature and recovery of defects were investigated.