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Measurement of Carbon Diffusion Coeficient - Calibration of Sputter Depth
Král, Lubomír ; Čermák, Jiří
Depth profiling mode of MiniSIMS device was applied to diffusion measurement. Calibration of crater depth was done using shearing interference microscope Zeiss Epival Interphako (ZEI) and confocal mikroskope Olympus LEXT OLS3100 with atomic force microscopy (AFM) modul. The ZEI uses one of the classical interferometric measuring methods. Generally this method leads to results with considerable experimental error. AFM is a very high-resolution type of scanning probe microscopy, with typical resolution of the order of fractions of nanometers, which is more than 1000 times better than the optical diffraction limit. However, the results taken by ZEI were in agreement with much more precise results of surface profiling achieved by AFM. It was found, at given experimental conditions (Fe-rich matrix, Ga + primary ions, 5 kV/3nA, DWT=1), that the sputter rate is some 0.3 nm per a single sputter scan of the crater area (50x50 µm). This depth calibration with SIMS technique can be applied to the study of carbon diffusion in BCC iron as an example. Special technique was developed, which avoids radio-tracer measurements with C-14. Obtained results are lower than the extrapolated values, which may be due to limited solubility of carbon in iron.
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Hydrogen Storage Capacity of Mg/Mg2Ni Eutectic Doped with Elements from Groups XIII and XIV
Čermák, Jiří ; Král, Lubomír
In the present paper, the chemical composition of Mg-8.5 at.% Ni-2.7at.%X alloys (X – elements of the 13th and 14th groups) as prospective hydrogen storage was investigated. Experimental alloys were studied in three states: (i) after stabilization anneal, (ii) after stabilization anneal and hydrogen charging, and (iii) after stabilization anneal, hydrogen charging and hydrogen desorption. It was ascertained that a ratio of concentration of X in two principal phases – Mg2NiH4(-X) and MgH2(-X) – was a decreasing function of the ionization potential of X. The stronger the preference of X for Mg2NiH4-X phase, the higher the hydrogen storage capacity of Mg-Ni-X alloy was. For X = In, the hydrogen storage capacity was slightly higher than the capacity of an un-alloyed binary eutectic Mg-Ni alloy.
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Improvement of Hydrogen Desorption Characteristics of Eutectic Mg/Mg2NiH4 and Mg2NiH4 by In addition
Čermák, Jiří ; Král, Lubomír
Mg-xNi alloys are known as perspective hydrogen storage materials [1,2]. Hydrogen storage capacity and hydrogen desorption rate of binary alloys Mg-Ni are, however, still unsatisfactory and therefore, improvements are sought, e.g., by introduction of a proper catalyst [3]. As candidate elements, transition metals [4] are often used that attract bonding valence electrons and, hence, destabilize the hydrides. However, also elements with weaker bond to H than that of Mg, or even non-hydride forming elements show a beneficial effect upon the hydrogen desorption rate [5,6]. The present investigation continues our previous work [7,8]. Here we investigate the resistance of eutectic Mg/Mg2Ni against the poisoning by residual air and possible ways how to improve the hydrogen desorption kinetics of Mg2NiH4 by doping. As dopants, elements of the 13th and the 14th group were tested that do not form stable hydrides.
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Impact of Heat Treatment Environment of Microstructure and Transformation Path in NiTi Shape Memory Alloy
Kuběnová, Monika ; Zálešák, Jakub ; Čermák, Jiří ; Barták, Tomáš ; Dlouhý, Antonín
We report results of differential scanning calorimetry (DSC) experiments in which heat flow (T) from and to Ti-50.9at%Ni shape memory samples was recorded during the temperature scan through a B2 B19’ transformation range. Prior to the DSC experiments, the samples were separately annealed in evacuated quartz capsules containing different hydrogen and helium mixtures with an overall filling pressure of 900 mbar. The quartz tubes containing the annealed samples were subsequently quenched into cold water. After quenching, the capsules were opened, martensitic transformations were investigated by DSC and the microstructure of the samples was assessed by transmission electron microscopy (TEM). Annealing in the mixtures with an increasing partial pressure of hydrogen led to a considerable drop in the latent heat associated with the B2 B19’ martensitic transformation. Results obtained using TEM suggest that hydrogen may function as a catalytic substance that accelerates the long range ordering of Ni atoms in early stages of Ni4Ti3-phase precipitation. The selected area diffraction study focused on patterns in <100>B2 and <110>B2 zones and provided evidence for diffuse scattering due to spatial modulations of the lattice constant. These variations in the background electron intensities might be related to a precursor of Ni4Ti3 phase in its early state of formation.
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Creep in NiAl-Mo Eutectics
Dudová, Marie ; Barták, Tomáš ; Kuchařová, Květa ; Dlouhý, Antonín
We report on creep in NiAl-Mo ternary eutectic and NiAl intermetallic, having respective nominal compositions Ni-45.5Al-9Mo and Ni-45.2Al (at.%). These alloys were directionally solidified in a high-temperature optical floating zone furnace. The eutectic alloy exhibited a well-aligned rod-like microstructure, consisting of NiAl matrix and 14% (by volume) continuous Mo-fibres oriented along a [001]-crystal growth direction. Cylindrical [001]-oriented specimens were loaded in compression at temperatures in a range 1073 – 1173 K. Formidable strengthening by regularly distributed fine fibres (typical diameter, 400 nm) was observed which resulted in minimum creep rates of the NiAl-Mo eutectic that were seven orders of magnitude lower than the corresponding minimum creep rates of the NiAl matrix. Preliminary microstructural investigations suggested that the strengthening effect is due to an interaction between Mo fibres and subgrain boundaries that form in the course of creep. This interaction leads to an increase of dislocation density in the vicinity of fibres and to an efficient redistribution of stresses in the microstructure.
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Influence of Heat Treatment on Microstructure and Transformation Characteristics of NiTi Shape Memory Wires
Zálešák, Jakub ; Kuběnová, Monika ; Čermák, Jiří ; Svoboda, Milan ; Dlouhý, Antonín
The present study shows how heat treatments affect microstructure and transformation behaviour of superelastic Ni-rich NiTi shape memory wires. Wire samples were sealed into quartz tubes, filled with hydrogen reduction atmosphere, heated for 10 minutes at temperatures increasing in a range from 500 to 600°C and subsequently quenched into cold water. Characteristic transformation temperatures MS, MF, AS, AF, thermal hysteresis and latent heats were investigated using differential scanning calorimetry (DSC). We observed significant changes in DSC charts which recorded B2 → R and R → B19‘ phase martensitic transformations. Increasing temperature of the heat treatment resulted in a convergence of the two transformation peaks. R-transformation commenced at systematically lower temperatures and the beginning of the B19‘ transformation was shifted to higher temperatures with increasing temperature of the heat treatment. In parallel, latent heat of the overall B2 → B19‘ transformation clearly increases. We rationalize these significant changes in the transformation behaviour on the basis of the microstructural development during the heat treatment which is characterized by means of SEM, TEM and EBSD techniques.
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Compressive Creep Tests of An Aluminium Powder Composite Reinforced by Ceramic Particles
Dvořák, Jiří ; Král, Petr ; Balog, M. ; Simančík, F. ; Sklenička, Václav
The aim of this work is to study of a composite mixture of aluminium powders, to analyze of composite microstructure and mostly to describe the creep behaviour of composite in compression. The experimental material was based on Al powder matrix (Al 99%) about the particle size of less than 200 µm. This powder was mixtured with silicon carbide particles (SiC) having the size about 10 µm. The Al composite powder was prepared via conventional direct hot-extrusion (DE) at temperature 450°C. The microstructural investigations were performed using OM and SEM. It was found that DE process exhibits some breaking of carbide particles to size of range from 0.5 to 5 µm. Creep tests in compression were conducted at temperatures 423 -623 K and at applied stresses in the range from 60 to 100 MPa. Consequently, for an evaluation of controlling creep mechanisms an activation energy of creep and the stress exponent of the creep rate were determined.
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Changes of Phase Composition of NaAlH4 Based Complex Hydrides
Roupcová, Pavla ; Schneeweiss, Oldřich
The Mössbauer study is target to valence of Fe-doped phase and its changes during preparation by mixing with NaAlH4 and charging and discharging cycles. The 2 mol % FeCl2·4H2O powder was contained in the asmixing material. The dry milled sample did not transformed during the milling in the protective atmosphere. The significant change was approved in the firstly hydrogenation step only. The analysis shows FeClO which released the most significant component in the dehydrogenation and hydrogenation steps. The amount of FeClO was decreased with the all following step of hydrogenation and dehydrogenation. The fine paramagnetic particles of iron oxides were detected and their amount increased influenced of gas impurities. The longer period of heat treatment shows the agglomeration of iron oxides and their magnetic effect.
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Fatigue strength of wheathering steel ATMOFIX 52A
Kunz, Ludvík ; Vlk, M. ; Zavadilová, Petra ; Klusák, Jan ; Navrátilová, L.
Deterioration of fatigue properties of weathering steels is a serious problem of operating life of engineering components subjected to corrosion and cyclic loads. There are two possible mechanisms of damage, which are discussed in literature. There is an effect of surface roughening, which develops during corrosion, and an effect of corrosion cracks, which can influence the fatigue crack initiation. The paper contains results of an experimental determination of fatigue life of ATMOFIX 52A grade steel with a corroded surface and comparison with the fatigue strength of basic smooth material. The notch effect of corrosion dimples, which initiated fatigue cracks, was determined on the basis of fractographic observation and numerical evaluation of stress concentration. It has been found that the reduction of the fatigue life can be quantitatively well predicted by means of the fatigue notch effect of corrosion dimples. No risky corrosion cracks were found in the studied corroded material
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Investigating ground state of nickel nitrides NiN and Ni2N with the help of quantum-mechanical calculations
Elstnerová, P. ; Friák, Martin ; Šob, Mojmír ; Neugebauer, J.
We have employed quantum mechanical calculations to identify ground-state structures of nickel nitrides NiN and Ni2N for which experimental data are lacking. In total 19 crystalline phases have been calculated for which not only thermodynamic but also structural and selected elastic properties have been determined. Employing density functional theory (DFT) methods, the total energies were calculated by means of a pseudopotential approach implemented in the VASP code and selected states were benchmarked by the full-potential linearized augmented plane wave (FP-LAPW) method implemented in the WIEN2k code. For the exchange-correlation energy the generalized gradient approximation (GGA) has been used.
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