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PROPERTIES OF NANOCRYSTALLINE FE-NI PARTICLES PREPARED BY THERMAL REDUCTION OF OXALATE PRECURSORS
Švábenská, Eva ; Roupcová, Pavla ; Havlíček, Lubomír ; Schneeweiss, Oldřich
Recent technological advancements require development of cost-effective and high-performance magnets \nwhich ideally do not contain rare earth metals or noble metals. The promising candidates are Fe-Ni-based \nalloys, in particular, the Fe50Ni50 L10 phase (tetrataenite), which has a great perspective for producing hard \nmagnetic materials. Our study explores a promising method for preparing nanoparticles of Fe-Ni alloy from an \niron-nickel oxalate precursor. The coprecipitation method was employed to prepare oxalate precursors, \nfollowed by controlled thermal decomposition in a reducing hydrogen atmosphere. The morphology and \nproperties of the resulting particles were analysed using scanning electron microscopy (SEM) coupled with \nenergy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Mössbauer spectroscopy (MS), and \nmagnetic measurements.\nThe SEM analysis revealed that the particles have approximately cube-shaped unit cell morphology with a\nsize in a range of 1 - 2 μm. Upon annealing, the samples contain multiple phases with varying Fe-Ni content.\nMagnetic measurements confirmed the formation of magnetically suitable Fe-Ni phases in the samples after \nannealing. Mössbauer spectroscopy emerged as a highly effective method for characterizing individual phases \nof the Fe-Ni system.
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Reaction synthesis of bulk intermetallic materials from kinetic spraying deposits
Stejskal, Pavel ; Roupcová, Pavla (referee) ; Jan, Vít (advisor)
This work deals with issues of preparation of intermetallics based on iron, nickel and titanium aluminides. It works with an idea of preparation of bulk material by reaction synthe-sis from kinetic spraying deposits by cold spray. Theoretical part is concerned with phases and compounds of these aluminides for structural applications, their characteristics and present fabrication. In experimental part there are studied microstructures created by annealing of deposits.
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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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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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MICROSTRUCTURE AND COMPOSITION OF FINE PARTICLES RELEASED BY CAR BRAKING
Švábenská, Eva ; Roupcová, Pavla ; Pizúrová, Naděžda ; Schneeweiss, Oldřich
Vehicular traffic is connected with large volume of fine particles released during brake processes of cars. Our research is focused on the phase, structure and chemical analysis of the fine particles taken from some car brake parts by their services. The information on structure and phase composition was obtained by X-Ray Powder Diffraction, Mossbauer Spectroscopy, scanning electron microscopy with EDX and transmission electron microscopy. The results of the wear debris analysis are compared with original brake materials components. Most of recognized particles are based mainly on iron oxides. Wear brake particles are discussed in the relation to the potential risk to the environment and human health.
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MICROSTRUCTURE AND COMPOSITION OF FINE PARTICLES RELEASED BY CAR BRAKING
Švábenská, Eva ; Roupcová, Pavla ; Pizúrová, Naděžda ; Schneeweiss, Oldřich
Vehicular traffic is connected with large volume of fine particles released during brake processes of cars. Our research is focused on the phase, structure and chemical analysis of the fine particles taken from some car brake parts by their services. The information on structure and phase composition was obtained by X-Ray Powder Diffraction, Mossbauer Spectroscopy, scanning electron microscopy with EDX and transmission electron microscopy. The results of the wear debris analysis are compared with original brake materials components. Most of recognized particles are based mainly on iron oxides. Wear brake particles are discussed in the relation to the potential risk to the environment and human health.
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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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Nanoscale phases on surface Fe-6Si magnetic sheets
Švábenská, Eva ; Roupcová, Pavla ; Král, Lubomír ; Bulín, Tomáš ; Vondráček, Martin ; Foldyna, Josef ; Čechal, J. ; Schneeweiss, Oldřich
Analysis of the nanoscale phases which appear on the surface Fe-6Si samples were carried out after the various treatments – grinding and etching, annealing, and water jet abrasion. The basic information on structure, chemical and phase composition was obtained by X-Ray Powder Diffraction (XRD), Scanning Electron Microscopy with EDX, Glow Discharge Optical Emission Spectrometry (GDOES), Mössbauer Spectroscopy and X-ray Photoelectron Spectrometry (XPS). The results show high stability of the surface phase composition after the mechanical and heat treatments. Results obtained from the surface analysis in micrometer depth (XRD, EDX, GDOES) do not show any changes after the different treatments. Iron oxides were detected in XPS and conversion electron Mössbauer spectra (CEMS) which analyze the surface composition in a nanometer scale. In addition to, fine changes in atomic ordering on the surface can be observed after mechanical and heat treatments in the CEMS spectra.
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