Papers by Author: Ivana Stulíková

Abstract: This work is focused on development of microstructure and properties of Mg-Y-Zn and Mg-Y-Nd-Zn alloys during heat and mechanical treatment. In the as-cast state both alloys exhibit almost equiaxed grains with little larger size in Mg-Y-Zn alloy and grain boundaries decorated by different structures - long period ordered structure (LPSO) was detected in Mg-Y-Zn alloy and eutectics of Mg₃Nd type structure in alloy with Nd addition. A high density of stacking faults is evident in both alloys. Both alloys were repeatedly isochronally heat treated from room temperature up to 440 °C. Resistivity and microhardness measurement was performed after each heating step. Stacking faults persist both annealings in both alloys and microhardness development shows no remarkable differences. LPSO in Mg-Y-Zn alloy disappears after the first annealing and was again detected after repeated annealing up to 340 °C. After the whole treatment no grain growth appeared. Differential scanning calorimetry measurement was performed at both repeatedly heated alloys up to 540 °C. There are three exothermic peaks in DSC curves of Mg-Y-Zn alloys that can be ascribed to embedding solute atoms in stacking faults, LPSO development and transformation and coarsening of grain boundary particles. DSC curves of Mg-Y-Nd-Zn alloy exhibit two exothermic peaks that probably correspond to precipitation of basal plates of γ ́and γ phase. Measurement of microhardness was performed after sequential deformation of both alloys in the as-cast state. The alloys were cold rolled in steps of 0,9 % thickness reduction up to cracks formation. Strengthening of both alloys is very similar but formation of cracks in the alloy with Nd addition begins after a lower reduction (about 11 %) compared to Mg-Y-Zn alloy (about 15 %).

Abstract: The Mg-Zn-Y system attracts interest of researchers due to the formation of quasicrystalline particles which are believed to improve mechanical properties of Mg-based alloys. In the Mg-Zn-Y-Nd-Zr alloy (WE43 modified by addition of Zn) studied here the formation of icosahedral phase (I-phase) with quasicrystalline structure competes with cubic W-phase. Grain boundary phases in Mg-Zn-Y-Nd-Zr alloys subjected to various heat treatments were characterized. It was found that the portion of the I-phase in Mg-Zn-Y-Nd-Zr alloy can be increased by a suitable heat treatment. Moreover, the solidification process is influenced by the cooling rate resulting in a striking difference in the morphology of grain boundary phases.

Abstract: The Mg-10 wt. % Gd and Mg-15 wt. % Gd alloys produced by squeeze casting were solution treated at 500 °C for 8 hours and subsequently naturally aged for more than 2 months. Electrical resistivity of both materials measured at 77 K decreases, if the alloys are kept at room temperature after quenching from the solution temperature. This change accompanied by a microhardness increase almost saturates after 2 months and is caused most probably by solute atoms clustering. Phase transformations and microhardness changes were investigated during isochronal annealing in both naturally aged alloys in comparison to just solution treated ones. Electrical resistivity changes measured at 77 K were used to characterize microstructure development. Transmission electron microscopy was performed at selected states heat treated in the identical way. The Mg15Gd supersaturated solid solution isochronally annealed up to 500 °C immediately after the solution treatment decomposes into following successive phases: β ́ ́ (D0₁₉) metastable → β ́ (cbco) metastable → β (Mg₅Gd) stable. All three possible orientation relationship modes of the metastable β ́ (cbco) phase existed at lower temperatures (up to 280 °C) but only one mode persists up to 330 °C. Precipitation of the β ́ (cbco) phase has not been observed in the Mg10Gd alloy annealed isochronally immediately after the solution treatment. The natural ageing does not change the precipitation sequence but concentration of Gd atoms involved in individual precipitation processes is influenced in both alloys. Peak hardening increases after natural ageing in the Mg15Gd alloy, shifts to higher temperatures and the temperature region of peak hardening extends.

Abstract: Hydrogen interaction with vacancies and dislocations in Pd were investigated in the present work. Well annealed and plastically deformed Pd samples were electrochemically doped with hydrogen up to various hydrogen concentrations. Subsequently the samples were subjected to linear annealing (10 K/min) and hydrogen desorption was studied by differential scanning calorimetry (DSC). An endothermic peak caused by hydrogen desorption was observed in the DSC curve of well annealed sample at ∼ 178 °C. In plastically deformed samples this peak is shifted to higher temperatures since hydrogen is trapped at dislocations and its diffusivity is suppressed. Moreover, it was found that if the atmosphere surrounding the heated sample contains oxygen the endothermic hydrogen desorption peak is followed by a strong exothermal peak caused by fusion of desorbed hydrogen with oxygen into water vapour molecules. To avoid this undesired effect DSC measurements have to be done in a protective atmosphere which does not contain oxygen.

Abstract: The effect of cold-rolling on mechanical and electrical properties, microstructure and recrystallization behaviour of the AlMn, AlScZr and AlMnScZr alloys was studied. The materials were investigated during isothermal annealing at 300, 400, 500 and 550°C and during step-by-step quasilinear annealing from 200°C up to 600°C with a heating rate of 100 K/h followed by subsequent isothermal annealing at 600°C/5 h. Precipitation reactions were studied by electrical resistometry and (micro) hardness measurements. The microstructure development was investigated by electron microscopy and electron backscatter diffraction examinations. The hardening effect is due to uniformly distributed Al₃Sc and/or Al₃(Sc,Zr) particles. The distinct changes in resistivity of the alloys above ∼ 300°C are mainly caused by precipitation of Mn-containing particles. It has a negligible effect on hardness. Phase transformations in the AlMn and AlMnScZr alloys are highly enhanced by cold rolling. The precipitation is dependent on the deformation degree – the more deformation the more intensive precipitation of the Mn-containing particles. The combination of Mn, Sc and Zr additions to Al substantially suppresses recrystallization at 550°C. A partial recrystallization was observed in the AlScZr alloy and AlMnScZr alloy after annealing 550°C/60 min and 550°C/760 min, respectively. The decomposition sequence of the supersaturated solid solution of the AlMnScZr alloy is compatible with the decomposition sequence of the AlScZr system accompanied and/or followed by the formation of Mn-containing particles.

Abstract: Response to isochronal annealing up to 440°C was investigated in squeeze cast Mg2Y1Zn alloy and in the same alloy prepared by powder metallurgy and extrusion at 280°C (PM). Electrical resistivity measurements at 77 K and at room temperature after each annealing step and differential scanning calorimetry performed at various heating rates characterized phase changes proceeding during the heat treatments. Transmission and scanning electron microscopy and optical microscopy revealed ribbons of a long-period ordered structure and a relatively high density of stacking faults in grain interiors of the cast alloy having the grain size of ~50 μm. Well pronounced subgrains were observed in the PM prepared alloy. Secondary phase particles decorate grain boundaries in this alloy. Electrical resistivity response of the cast alloy to isochronal annealing up to 440°C shows three precipitation processes, whereas one significant process was revealed in the PM alloy. Activation energies of precipitation processes were determined. Microhardness exhibits good thermal stability in the whole temperature range in the cast alloy and up to 360°C in the PM alloy.

Abstract: The effect of hot extrusion at 350°C on microstructure, thermal, electrical and mechanical properties of the AlMnScZr alloy was studied. The samples of the cast and of the hot-extruded alloys were annealed from 20°C up to 600°C. Transmission and scanning electron microscopy and electron backscatter diffraction examinations of specimens quenched from temperatures of significant resistivity changes were used to identify microstructural processes responsible for these changes. The cast as well as hot-extruded alloy is characterized by a dispersion of fine coherent Al₃Sc and/or Al₃(Sc,Zr) particles, and furthermore the fine (sub) grain structure was observed in the hot-extruded alloy. Microhardness HV1 and resistivity values reflect different microstructure of the alloys accordingly. The distinct resistivity changes of the alloys are mainly caused by precipitation of Mn-containing particles. The apparent activation energy for the Al₆Mn-phase precipitation in the hot-extruded alloy was also determined. The obtained results agree with those observed in the alloys prepared by powder metallurgy studied in our previous work.

Abstract: Successive precipitation processes in solution treated Mg3Y3Nd alloy were studied by electrical resistometry, by differential scanning calorimetry and by microhardness. The results were compared to those in the commercial WE43 alloy. Five various phases known from the Mg-Gd-and Mg-Nd-type decomposition sequences form, dissolute or transform in the Mg3Y3Nd alloy. The main difference in the WE43 precipitation sequence is the absence of the β₁ phase particles. Electron microscopy confirmed that not the phase type of hardening particles but their morphology, size and orientation to the matrix determine the hardening effectiveness. Differential scanning calorimetry revealed exothermic effects connected to precipitation processes. Apparent activation energies of individual precipitation processes correspond to those in the MgTbNd and in MgNd alloys.

Abstract: Early stages of precipitation were investigated in solution treated binary Mg-Tb and Mg-Gd alloys. The supersaturated solid solution of Gd (or Tb) in Mg was formed by fast quenching of the alloys from solution treatment temperature. Decomposition of the supersaturated solid solution and precipitation effects were investigated by positron lifetime spectroscopy combined with microhardness testing. During solution treatment at elevated temperature some thermal vacancies form pairs with solute atoms. In quenched samples free vacancies are quickly annealed out, while more stable vacancies bound to solute atoms remain in the sample and enhance the diffusivity of solutes. The hardness of solution treated Mg-Tb and Mg-Gd alloys aged at ambient temperature rises due to formation of small clusters of Tb and Gd atoms. Isochronal annealing of Mg-Tb and Mg-Gd alloys leads to precipitation of coherent β phase, semicoherent β phase and incoherent β phase particles. It was found that natural aging of Mg-Tb alloy at ambient temperature has beneficial effect on subsequent hardening by β phase particles formed during annealing.

Abstract: Precipitation effects in age-hardenable Mg-13wt.%Tb alloy were investigated in this work. The solution treated alloy was subjected to isochronal annealing and decomposition of the supersaturated solid solution was investigated by positron annihilation spectroscopy combined with transmission electron microscopy, electrical resistometry, differential scanning calorimetry and microhardness measurements. Peak hardening was observed at 200°C due to precipitation of finely dispersed particles of β phase with the D0₁₉ structure. Vacancy-like defects associated with β phase particles were detected by positron annihilation. At higher temperatures precipitation of β and subsequently β phase takes place. Formation of these phases lead to some additional hardening and introduces open volume defects at precipitate/matrix interfaces. To elucidate the effect of plastic deformation on the precipitation sequence we studied also a Mg-13wt.%Tb alloy with ultra fine grained structure prepared by high pressure torsion. In the ultra fine grained alloy precipitation of the β phase occurs at lower temperature compared to the coarse grained material and the peak hardening is shifted to a lower temperature as well. This effect can be explained by enhanced diffusivity of Mg and Tb atoms due to a dense network of grain boundaries and high density of dislocations introduced by severe plastic deformation. Moreover, dislocations and grain boundaries serve also as nucleation sites for precipitates. Hence, precipitation effects are accelerated in the alloy subjected to severe plastic deformation.