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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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HYDROGEN SORPTION IN ORDERED Mg-In ALLOYS
Čermák, Jiří ; Král, Lubomír ; Roupcová, Pavla
Hydrogen storage (HS) performance of three Mg- x In- y CB alloys (CB - amorphous carbon, x = 55, 64, 73 y =\n10 wt%) was studied. Indium concentration covered an area of ordered β structures. Alloys were prepared by\nball-milling in hydrogen atmosphere. Kinetic curves and PCT isotherms were measured in the temperature\ninterval from 200 °C to 325 °C. X-ray diffraction spectroscopy (XRD) was used for structure investigation. Alloy\nwith x = 73 wt% In ( β ’’ structure) showed reversible amorphization during temperature cycling between about\n100 °C and 350 °C. Hydrogen sorption experiments were done by the Sieverts method under the hydrogen\ngas pressure ranging from 0.1 MPa to 2.5 MPa. It was found that hydrogen sorption capacity varied between\n0.47 and 1.1 wt% H 2 . Hydride formation enthalpy ∆H calculated from desorption PCT experiments was\nsignificantly lower than ∆H , known for pure Mg. This invoked an idea that atomic order of Mg-based HS\nmaterials might decrease the high thermodynamic stability of hydride phase.
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INFLUENCE OF GRAPHITE UPON THE KINETICS OF HYDROGEN SORPTION IN Mg@Mg17Al12
Čermák, Jiří ; Král, Lubomír ; Roupcová, Pavla
Influence of graphite addition to the ball-milling charge composed of Mg splinters and Mg17Al12 particles upon the hydrogen sorption was investigated at sorption temperature 623 K. Measurements were carried out by Sieverts method. Graphite facilitates the ball-milling: It prevents re-agglomeration of crushed particles into large secondary particles. It also suppresses sticking the milled material to the balls and walls of the milling jar. It was found that an increase of carbon concentration up to a certain limit c(L) lying between 14 and 23 wt. % C, carbon increases both the absorption and the desorption rates and hydrogen storage capacity. Above c(L), carbon causes a considerable decrease in HS capacity, which spoils the application potential of Mg@Mg17Al12/C. Crystallite size of the material under study, obtained by XRD, is in the order of tens of nm.
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HYDROGENATION OF CHOSEN MgMXN INTERMETALLICS (X=Al, Ga, In, Si, Sn)
Čermák, Jiří ; Král, Lubomír ; Roupcová, Pavla
Hydrogen sorption in chosen intermetallics MgmXn (Mg17Al12 , Mg2Ga, mixture of beta-Mg-In phases, Mg2Si and Mg2Sn) formed by magnesium and elements from the 13 th (X: Al, Ga, In) and 14 th (X: Si, Sn) groups was studied between the room temperature and T = 350 °C. Hydrogen pressure p varied from 10-3 MPa to 6 MPa.\nHydrogen solubility in alpha phase (solid solution of hydrogen in MgmXn before the hydride phase was nucleated) was close to hydrogen solubility in pure Mg. Concentration cH of hydrogen solved in Mg m X n depended linearly on pressure p , dependence of cH on temperature T was relatively weak. MgH2 was the main hydrogen storage phase in all the compounds MgmXn . Nucleation of MgH2 at 350 °C was observed at pressure above approximately 1 MPa in Mg17Al12 and above 2 Ma in other compounds. Maximum values of c H in hydride-containing compounds MgmXn detected at T = 350 °C depended on the stability of MgmXn .
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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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Detekce poškození Mg slitin nelinearní ultrazvukovou spektoskopií
Kober, Jan ; Převorovský, Zdeněk ; Trojanová, Z.
Na plochých zkušebních tělesech z hořčíkových slitin byl metodou nelineární ultrazvukové spektroskopie (NEWS) testován výchozí stav různě připravených vzorků. K nedestruktivnímu hodnocení byla použita dvou-frekvenční NEWS metoda - nelineární vlnově modulační spektroskopie (NWMS). Na základě spekter naměřených signálů byly vyhodnocovány nelineární parametry. Získané parametry byly porovnány s výsledky vizuálního pozorování zkušebních těles na výskyt defektů a s výsledky metalografické analýzy a byla diskutována jejich závislost.
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