Institute of Physics of Materials

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2023-11-12
00:02
NANOCERIA PREPARED BY ELECTRON BEAM EVAPORATION
Pizúrová, Naděžda ; Hlaváček, A. ; Kavčiaková, Zuzana ; Roupcová, Pavla ; Kuběna, Ivo ; Buršík, Jiří ; Sokovnin, S. Y.
Cerium oxide nanoparticles (nanoceria) are currently one of the most investigated nanomaterials because of their attractive properties used in biomedical applications, catalysis, fuel cells, and many others. These attractive properties are connected with the Ce3+ and Ce4+ valency state ratio. In the nanoparticle form, cerium oxides contain a mixture of Ce3+ and Ce4+ on the nanoparticle surfaces. Switching between these two states requires oxygen vacancies. Therefore, nanoceria's inherent ability to act as an antioxidant in an environmentally-dependent manner and a “redox switch” to confer auto-regenerating capabilities by automatically shifting between Ce4+ and Ce3+ oxidation states is significantly affected by surface morphology. Regarding this demanded behavior, we aimed to characterize synthesized nanoparticle surface quality and its influence on the cerium oxidation states. The received results were used to evaluate the synthesis method's suitability for suggested utilization. We used nanoparticles prepared by electron beam evaporation. This unique physical method includes nanoparticle creation through the fast cooling process followed by breaking radiation damaging nanoparticle surfaces to create surface off-stoichiometry. We prepared a sample containing clusters of a mixture of ultra-small nanoparticles and approximately 100 nm particles. X-ray diffraction confirmed the CeO2 phase in both components. To extract the finest component, we used centrifugal size fractionation. We received 200 nm clusters of 2-10 nm nanoparticles. Nanoparticle shapes and facet types were analyzed using transmission electron microscopy methods. We found out most nanoparticles were formed with truncated octahedrons containing {1,1,1} and {1,0,0} facet types and truncated cuboctahedrons containing {1,1,1}, {1,0,0}, and additional {1,1,0} facets. No octahedron (without truncation) containing only {1,1,1} facets was observed. Nanoparticle shapes containing {1,1,0} and {1,0,0} are suitable for redox activity. Some amount of irregular shapes, beneficial for redox activity, was also observed. Spectroscopy methods confirmed Ce3+ content.

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2023-10-16
21:27
Influence of severe plastic deformation and subsequent annealing on creep behaviour of martensitic 9% Cr steel
Král, Petr ; Dvořák, Jiří ; Sklenička, Václav ; Horita, Z. ; Tokizawa, Y. ; Tang, Y. ; Kunčická, Lenka ; Kuchařová, Květa ; Kvapilová, Marie ; Svobodová, M.
The objective of the study is to evaluate the effects of severe plastic deformation (SPD) and annealing on creep behaviour of advanced tungsten modified creep-resistant 9 % Cr martensitic P92 steel. The as-received P92 steel was deformed by high-pressure torsion (HTP), high-pressure sliding (HPS) and rotary swaging (RS) at room temperature prior creep testing. These SPD methods imposed significantly different equivalent plastic strain in the range from 1 up to 20. Constant load creep tests in tension were performed in an argon atmosphere at 873 K and applied stress ranging from 50 to 200 MPa. The microstructure and phase composition of P92 steel were studied using a scanning electron microscope Tescan Lyra 3 and a transmission electron microscope Jeol 2100F. The results show that under the same creep loading conditions the HPT and HPS-processed P92 steel exhibited significantly faster minimum creep rates, creep fracture strain and the decrease in the value of the stress exponent of the creep rate in comparison with as-received P92 steel. However, it was revealed that the RS-processed specimens exhibited one order of magnitude lower minimum creep rate and lower ductility compared to commercial P92 steel. The creep curves for the HPT and HPS-processed states exhibited a pronounced minimum of strain rate. The pronounced minimum of strain rate disappeared when these states were annealed at 923K/500h before application of creep loading. The microstructure changes occurring during creep and different creep behaviour between as-received and deformed states are discussed.

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2022-12-25
22:33
Advanced statistical evaluation of fatigue data obtained during the measurement of concrete mixtures with various water-cement ratio
Seitl, Stanislav ; Benešová, A. ; Blasón, S. ; Miarka, Petr ; Klusák, Jan ; Bílek, V.
The Basquin’s law is usually applied for the evaluation of fatigue properties of civil engineering \nmaterials. For materials like concrete, some researchers recommended applying the Weibull model. In this\ncontribution, Basquin’s law, Castillo-Canteli model and Kohout-Věchet model were applied for the advanced \nstatistical description of S−N curves (Wöhler curve). For the application of the models, the experimental data \nmeasured on reference concrete mixtures used for the development of self-healing concrete at the Faculty of \nCivil Engineering, TU Ostrava. Fitting data of applied models were compared and analyzed

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2022-11-20
00:00
AB INITIO STUDY OF SILVER NANOPARTICLES, GRAIN BOUNDARIES AND THEIR \nQUADRUPLE JUNCTIONS
Polsterová, S. ; Všianská, Monika ; Friák, Martin ; Pizúrová, Naděžda ; Sokovnin, S. ; Šob, Mojmír
Motivated by our experimental research related to silver nanoparticles with various morphologies, we have employed quantum-mechanical calculations to provide our experiments with theoretical insight. We have computed properties of a 181-atom decahedral silver nanoparticle and two types of internal extended defects, -5(210) grain boundaries (GBs) and quadruple junctions (QJs) of these GBs. We have employed a supercell approach with periodic boundary conditions. Regarding the thermodynamic stability of the decahedral nanoparticle, its energy is higher than that of a defect-free face-centered cubic (fcc) Ag by 0.34 eV/atom. As far as the -5(210) GB is concerned, its energy amounts to 0.7 J/m2 and we predict that the studied GBs would locally expand the volume of the lattice. Importantly, the system with GBs is found rather close to the limit of mechanical stability. In particular, the computed value of the shear-related elastic constant C66 is as low as 9.4 GPa with the zero/negative value representing a mechanically unstable system. We thus predict that the -5(210) GBs may be prone to failure due to specific shearing deformation modes. The studied GBs have also the value of Poisson’s ratio for some loading directions close to zero. Next, we compare our results related solely to -5(210) GBs with those of a system where multiple intersecting -5(210) GBs form a network of quadruple junctions. The value of the critical elastic constant C66 is higher in this case, 13 GPa, and the mechanical stability is, therefore, better in the system with QJs.

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2021-09-26
00:06
Structural and magnetic properties of Fe-oxide layers prepared by inkjet printing on Si-substrate
Zažímal, František ; Svoboda, T. ; Dzik, P. ; Homola, T. ; Jirásková, Yvonna
Magnetic films with two, four, six, and eight layers were prepared using 2D inkjet printing on the 333 K heated Si-substrates at ambient conditions. The microstructure, phase composition of layers, and magnetic studies were investigated using wide spectrum of experimental methods with the aim to find the optimal conditions for producing magnetic sensors by digital printing technology in the near future. As the magnetic compound, the hematite powder was chosen and its milling with Si-binder dissolved in dowanol using glass balls and vial to prevent contamination was done to prepared suspension appropriate for printing. It is shown that hematite transformed markedly into maghemite, thus the layers consisted of small amount hematite and dominant maghemite phases determining the magnetic properties. From the viewpoint of magnetic behavior, the highest saturation magnetization and the lowest coercivity was obtained at the sample with 8 layers.

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2021-03-28
00:00
WE43 BIOCOMPATIBLE ALLOY AFTER SEVERE PLASTIC DEFORMATION: STRUCTURE CHARACTERIZATION
Kunčická, Lenka ; Král, Petr ; Dvořák, Jiří ; Kocich, R.
The report presents results of the analyses of biocompatible WE 43 Mg-based alloy processed by friction stir processing (FSP) at two different rotational speeds of 400 RPM, and 1200 RPM. The structures were observed by scanning electron microscopy (SEM), electron backscattered diffraction (EBSD). Observations were primarily focused on characterizations of grains and textures, supplementary testing of mechanical properties was performed via tensile tests. The results of low angle grain boundaries fractions and grain sizes showed that both the processing methods led to significant grain refinement and recrystallization, the average grain diameter within the 1200 RPM sample was less than 2 μm. Texture observations showed slight tendencies of the grains to align in the {0001}〈101̅0〉 and {0001}〈112̅0〉 preferential orientations, however, the maximum intensities were only about two times random. Supplementary tensile tests confirmed the positive effects of FSP on structures and properties of both the samples.

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2021-02-24
00:44
PHASE COMPOSITION OF CHOSEN Mg-BASED MATERIALS DURING HYDROGEN SORPTION
Čermák, Jiří ; Král, Lubomír ; Roupcová, Pavla
Phase transformation during hydrogen sorption was investigated in ten chosen magnesium-based hydrogen storage (HS) materials. Chemical composition of the materials consisted of Mg, as a principal hydrogen-binding element, additive X and amorphous carbon (CB), as an anti-sticking component. In order to assess the effect of X itself upon the structure, values of concentration of both X and CB were fixed to about 12 wt. %. The influence of X = Mg2Si, Mg2Ge, Mg17Al12, Mg5Ga2, NaCl, LiCl, NaF, LiF and two combinations Ni+Mg17Al12 and Ni+Mg2Si upon the changes in phase composition was tested. Phase content in HS materials was observed (i) after the intensive ball milling (BM), (ii) after the BM followed by hydrogen charging at 623 K and (iii) after the BM and one hydrogen charging/discharging cycle (C/D) at temperature 623 K. The study was carried out by SEM and XRD. It was found that, the C/D is approximately structurally reversible for X = Mg2Ge, Mg17Al12, NaF and LiF. However, additives X = Mg17Al12 and NaF decompose already during the BM. In alloys with combination of Ni with Mg17Al12, new phases NimAln are formed. Phase composition changed during C/D for X = Mg2Si Mg5Ga2 and Ni+Mg2Si due to equilibration of phases composition. Observed structure changes of HS materials with chloride ionic additives NaCl and LiCl are, most likely caused by the relatively strong affinity between Mg and Cl. Hydrogen storage capacity of all studied alloys was 6.0 +/- 0.3 wt. % H-2.

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2021-02-24
00:43
Effect of casting conditions and heat treatment on high temperature low cycle fatigue performance of nickel superalloy Inconel 713LC
Šulák, Ivo ; Obrtlík, Karel ; Hrbáček, Karel
The present work is focused on the study of high temperature low cycle fatigue behaviour of Inconel 713LC produced by a vibratory investment casting (VIC) in as-cast conditions and in the condition after heat treatment (HT) consisting of hot isostatic pressing (HIP) followed by precipitation hardening. Low cycle fatigue tests were carried out on cylindrical specimens in symmetrical push-pull cycle under strain control with constant total strain amplitude and strain rate at 800 °C in air. Hardening/softening curves and fatigue life curves of both materials were assessed and compared with data of Inconel 713LC produced by a conventional investment casting (CIC). Cyclic hardening can be observed in the high amplitude domain while saturated stress response is apparent for low amplitude cycling for all material batches. Data presented in Basquin representation show an increase in fatigue life of both VIC batches compared to the CIC batch, however, no effect of HT on fatigue life of Inconel 713LC produced by VIC was observed. In contrast, the heat treated Inconel 713LC demonstrates slightly higher fatigue life in Coffin-Manson representation. The microstructure of both superalloys was studied by means of scanning electron microscopy (SEM). The microstructure of superalloy is characterized by dendritic grains with casting defects. It comprises the γ matrix, cubic γ´ precipitates, eutectics and carbides. The effect of the VIC and HT on fatigue performance and microstructure of Inconel 713LC is discussed.

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2020-12-03
22:56
Měření velmi pomalých creepových deformací materiálů pro pokrytí jaderného paliva technikou helikoidních vzorků.
Kloc, Luboš
Metodika umožňuje přímé experimentální stanovení creepových vlastností povlakových trubek jaderného paliva za podmínek, při kterých probíhá creepová deformace velmi pomalu, takže není standardními metodami creepových zkoušek měřitelná. Takto získané údaje jsou potřebné ve výpočtových kódech pro modelování chování paliva v reaktoru i mimo\nněj při skladování paliva a dosud chybí, popřípadě jsou získávany nespolehlivou extrapolací.

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2020-12-03
22:56
Snímání akustických emisí při zkoušce tečením (creepem) v ochranné atmosféře
Dvořák, Jiří ; Svobodová, M. ; Sklenička, Václav
Cílem vypracované metodiky snímání akustických emisí 'in-situ' v průběhu creepové zkoušky v ochranné atmosféře byla minimalizace či odstranění šumů na záznamech akustické emise způsobených synergicky působícími oxidačními procesy, které mohou kriticky ovlivňovat identifikaci a intenzitu působících vlastních creepových degradačních procesů a relevantní vyhodnocení naměřených dat.

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