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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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Corrosion of Nickel Exposed to LiF-NaF Molten Salt
Král, Lubomír ; Čermák, Jiří ; Matal, O. ; Šimo, T. ; Nesvadba, L.
This work is devoted to study of changes of structure and chemical composition in corrosion areas of the chosen candidate alloy, Nickel 201, for components of a LS-VHTR. The material was annealed at 1013K/10h/vacuum and at 1000°C/24h/Ar before corrosion tests. The annealed material was studied after its exposure to the molten mixture of 60 mol. % LiF + 40 mol. % NaF at the temperature of 1013K. The exposition was carried out in a quasidynamic regime, which simulates real circulation of the coolant (a mixture of molten salts) in the piping. The structure of the alloy was studied by SEM. Severe corrosion damage was observed in grain boundaries.
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Corrosion of chosen Ni-based material exposed to LiF-NaF molten salts
Král, Lubomír ; Čermák, Jiří ; Matal, O. ; Šimo, T. ; Nesvadba, L.
This work is devoted to study of changes of structure and chemical composition in the surface layer of chosen candidate alloy Ni – 6 W – 9 Mo – 1.7 Ti – 7 Cr (in wt. %) for components of a LS-VHTR. The material was studied after its exposure to molten mixture 60 mol. % LiF + 40 mol. % NaF at temperature 993 and 1013K. The exposition was carried out in a quasidynamic regime, which simulates coolant (the mixture of salts) natural circulation conditions in components. The structure of the alloy was studied by SEM. Severe corrosion damage was observed in the surface layer, which thickness was about 300 μm.
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Low-temperature diffusion of carbon in iron measured by SIMS technique
Čermák, Jiří ; Král, Lubomír
Depth profiling mode of MiniSIMS device was applied to diffusion measurement. As an example, carbon diffusion in BCC iron was studied. There are sparse experimental diffusion data at temperatures below the eutectic horizontal (996 K). This is caused by the fact that direct measurement of carbon diffusion coefficient in ferrite at low temperatures is complicated by very low solubility of carbon. For practical purposes, the extrapolation of high-temperature data to low temperature region is usually used for estimation of diffusioncontrolled kinetics in ferrite alloys. Present work has shown that the SIMS technique can be applied to the study of carbon diffusivity in iron. 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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Objemová kovová skla na bázi železa - optimalizace odlévání
Stloukal, Ivo ; Král, Lubomír ; Čermák, Jiří
V tom příspěvku byla studována slitina na bází Fe, která je perspektivní slitinou pro přípravu objemových kovových skel. Nominální složení bylo dáno následujícím vzorcem Fe.sub.56./sub.Co.sub.7./sub.Zr.sub.10./sub.Mo.sub.5./sub.W.sub.2./sub. B.sub.15./sub.. Byly aplikovány dvě licí metody: (i) konvenční lití do měděné kokily v indukční peci a (ii) odlití v obloukové peci. V prvním případě byl průměr ingotu 1 mm a ve druhém byla použita speciální dvoudílná kokila se vstupními otvory o průměrech 3 a 1 mm, respektive. Mikrostruktura připravených slitin byla studována optickou mikroskopií, SEM (skenovací elektronová mikroskopie) a XRD (rentgenová difrakce).
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Kinetika vodíku v Mg2Ni a v hydrogenovaném eutektiku Mg-Mg2Ni
Čermák, Jiří ; Král, Lubomír ; Stloukal, Ivo
V teplotním intervalu 552 - 723 K byla měřena teplotní závislost celkového množství vodíku desorbovaného z hydrogenovaného Mg a eutektika Mg-Mg2Ni (23,5 hm.% Ni). Experimenty byly prováděny v oblasti pod rovnovážným tlakem, kde tyto hydridy - perspektivní jako pevná media pro uchovávání vodíku - jsou nestabilní a proces desoprce je řízen hlavně difúzí vodíku v příslušném hydridu (MgH2 a/nebo Mg2NiH4). Difúzní koeficienty vodíku byly vyhodnoceny z desorpčních křivek and difúzní koeficinty vodíku podél mezifázové hranice MgH2/Mg2NiH4 byly odhanuty z výsledků získaných pro eutektickou slitinu.
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