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The influence of mechanical alloying on contamination of powder mixtures and bulk materials
Kubíček, Antonín ; Hadraba, Hynek (referee) ; Moravčík, Igor (advisor)
This thesis deals with the influence of process parameters on the contamination level of powder materials produced by mechanical alloying (MA) technology. For this purpose austenitic stainless steel 316 L and equiatomic CoCrFeNi high-entropy alloy (HEA) were prepared by high-energy ball milling. Both materials were milled in argon and nitrogen atmospheres from 5 to 30 hours. Spark plasma sintering method (SPS) was then used for consolidation of chosen powder samples. Chemical analysis of contamination within MA was carried out using combustion analysers for determination of carbon, oxygen, and nitrogen contents after different lengths of milling. Also differences in chemical composition of powder and corresponding bulk samples were measured. The microstructure analysis using scanning electron microscopy (SEM) of both powder and bulk materials was executed with focus on oxide and carbide presence and dispersion. Increasing content of carbon with increasing milling time was observed across all measured samples. This contamination is attributed to using milling vial made of tool steel AISI D2 (containing 1,55 wt. % of carbon). Increase of carbon content within consolidation using SPS was also observed. Milling of specimens using N2 as milling atmosphere caused higher contamination level in both AISI 316 L and HEA compared to milling in argon.
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High-entropy alloys – bulk alloys and surface treatments
Pišek, David ; Šiška, Filip (referee) ; Hadraba, Hynek (advisor)
Master‘s thesis deals with the preparation and evaluation single-phase high-entropy alloy based on cobalt, chromium, iron, nickel and manganese and its variants strengthened by dispersion of oxidic particles. High-entropy alloy was prepared in powder form by mechanical alloying from the equiatomic proportions of atomic powders. Obtained powder was subsequently compacted by spark plasma sintering. By the method of mechanical alloying were successfully prepared single-phase high-entropy alloy and its variant strengthened by dispersion of nanometric yttria oxides. It has been found that the oxide particles present in the microstructure of high-entropy alloy significantly block mobility of grain boundary and dislocation at elevated temperatures. As a result of this behavior were observed doubling of alloy strength and decreasing of creep rate at 800 °C.
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Nitride dispersion strengthened Cantor´s high entropy alloys
Havlíček, Štěpán-Adam ; Moravčík, Igor (referee) ; Hadraba, Hynek (advisor)
High Entropy Alloy (HEA) is a class of construction steels based on the mixing of five or more elements in approximately equimolar ratios. Despite the ambiguity of their future use, HEAs represent a significantly new group of construction materials that are currently receiving a great deal of attention. Single-phase HEAs fail when used at elevated tempera-tures. The improvement of their high-temperature resistance was achieved by introducing a dispersion of oxides Al2O3 and Y2O3. To generalize the positive effect of dispersions on the mechanical properties at elevated temperatures, particles of a similar nature were cho-sen. These were dispersed particles of nitrides: hardness-incompatible AlN and hardness-compatible BN. The particles were evenly distributed inside the alloys by mechanical al-loying and compacted by SPS (Spark Plasma Sintering). The new structural alloy reached a density higher than 96.5 % and brought an increase in yield strength at room tempera-ture of up to 67 % and 40 % at elevated temperatures, while maintaining a homogeneous distribution of input powders.
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Multicomponent Alloys Based on Immiscible Systems Prepared by Powder Metallurgy Route
Adam, Ondřej ; Svoboda, Jiří (referee) ; Sopoušek, Jiří (referee) ; Jan, Vít (advisor)
Immiscible alloys are a relatively well-known group of materials, however, they are still being intensively studied, especially from the point of view of heterogeneous materials with very good mechanical properties, but also electrical properties, for example. The main part of the research deals with cast materials, although in the case of immiscible alloys, there is a risk of liquid separation, which results in the loss of mechanical properties. This dissertation deals with the study of Cu-Fe-based immiscible alloys prepared by powder metallurgy methods. The theoretical part summarizes basic information about immiscible alloys, their microstructure, properties, and production options. The experimental part is first devoted to the choice of the suitable chemical composition of the studied alloys and subsequently to the optimization and influence of the mechanical alloying parameters on the properties of prepared powders. The main part of the experiments contains a complex structural, phase, and thermal analysis of Cu50Fe50 and Cu50(FeCo)50 alloys. In both alloys, a dual-phase ultrafine-grained microstructure was formed after sintering. The most significant of the presented results is the excellent resistance to grain coarsening compared to the other ultrafine-grained materials, where even after sintering at very high temperatures, the average grain size remained below 1 micron. The presumed reason is the immiscible nature of the studied alloys.
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Characterization of oxide dispersion strengthened alloys prepared from various precursor materials
Dobrovolný, Tomáš ; Havlík, Petr (referee) ; Moravčík, Igor (advisor)
Submitted master’s thesis studies the influence of input precursors (powders) on the resulting properties of prepared steels. When manufactured using the mechanical alloying method, the input powders can have a significant effect on the resulting properties. The austenitic steel 15-15Ti (1.4970) was chosen as the prepared alloy, which is gradually beginning to find application in nuclear energy. In this work, two approaches were used to produce this steel powder, firstly the production of an alloy from the precursor powder of austenitic steel AISI 304L and secondly the alloy was produced only from pure elements. For each of these methods, two different milling conditions were chosen. Thus, a total of four mixtures of 15-15Ti austenitic steel powders were produced, which were sintered into bulk materials using the SPS method. Mechanical properties of sintered specimens were tested by a tensile test and a hardness measurement by Vickers hardness test. At the same time, microstructure analysis using SEM and phase composition analysis by XRD were performed, both for prepared powders and for sintered bulks.
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High entropy alloy preparation by means of mechanical alloying
Gamanov, Štěpán ; Krajňáková, Petra (referee) ; Moravčík, Igor (advisor)
This thesis deals with topic of high entropy alloys. The teoretical part explains what are high entropy alloys, how are they different from conventional alloys, how is their chemical composition proposed and what potencial these alloys have. The experimental part describes procedures of preparation of three high entropy alloys witch consists of Co, Cr, Fe, Ni and Ti, where the concentration of all elements except Ti remains the same. These alloys were prepared via mechanical alloying and sintered by SPS process. Crucial part of this thesis is characterization of these three alloys with EDS and XRD supported by hardness measuring and tensile tests.
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In-situ Synthesised Intermetallic Compounds in Powder Materials
Hanusová, Petra ; Novák, Pavel (referee) ; Skotnicová, Kateřina (referee) ; Dlouhý, Ivo (advisor)
The mechanical treatment of solids is one of the most common and widely used operations. The volume of solids subjected to chemical treatment is very large too. Therefore, combining these two ways into one seems to be a logical solution. This method is called the mechanochemical processing of materials. Processing materials in this way has many advantages. On the one hand, this processing is economically as well as technologically feasible. Even the materials that not react together in conventional way can be prepare in this way. The mechanochemistry/mechanochemical synthesis utilizes the mechanical energy to activate chemical reactions and structural changes. The aluminothermic reduction reactions induced by the high – energy ball milling are gaining importance because of the potential applications like the synthesis of microcrystalline and nanocrystalline in – situ metal matrix composites. The mechanical activation of the chemical reactions by high energy ball milling often changes the reaction mechanism and produces metastable materials. Changes of reaction mechanisms during mechanical alloying on four different systems were studied. The system was based on this composition: Al - B2O3 - X (X = C, Ti, Nb, Cr). The possibility of another in – situ reactions during spark plasma sintering process (SPS) was also investigated. All systems were mechanically alloyed under the same conditions. After alloying, on each system scanning electron microscopy was performed and qualitative and quantitative analysis was performed using X-ray diffraction. The indentation hardness and the indentation modulus of elasticity were evaluated using nanoindentation. All analyzes were performed after mechanical alloying as well as SPS and the results were compared to each other. Based on the results, a change of reaction mechanisms was proposed for all systems. It has been found that metal matrix composites are formed and, when chromium is used, hybrid composite material reinforced with intermetallic phase and aluminum borate has been developed.
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Advanced Composite Structural Steels for Applications in Heavy Liquid Metals
Husák, Roman ; Haušild, Petr (referee) ; Vilémová,, Monika (referee) ; Hadraba, Hynek (advisor)
Doctoral thesis was focused on preparing of new advanced ODS steels for use in heavy metal liquids enviroments. Possibility of new course for creating oxide dispersion in microstructure was verified by the course of internal oxidation of elements. By the internal oxidation method were prepared new ODS steels strengthened by complex oxides which were created by elements of IIIB and IVB group of elements. Based on analysis of damage ODS steels in LBE were designed surface protection of ODS steel by the oxide layer. The ODS steel protected by oxide layer was subjected to a corrosion test in LBE. For the experiments were chosen class of chromium steels: ferritic-martensitic steel 9Cr1WMnVTa and ferritic steels 14CrWTi and 17Cr1Mo. Steels without oxide dispersion and steel strenghtened by the dispersion based on Y-Ti-O oxides were prepared. On the steels were made series of mechanic tests which should reveal the effectivity of oxide dispersion on the strenght of steel prepared by the internal oxidation method and by the direct addition of oxide elements. It was found that significantly harder oxide material couldn't be fully disrupted through the mechanical alloying and fine oxide dispersion couldn't be created. There was verified fine oxide dispersion could be created by the internal oxidation method and by the direct adding of oxide elements. Same kind of steels strenghtened by new kind of complex oxides based on Y, Ce, Hf, La, Sc and Zr were prepared. The chemical analyses have proven that all added elements could created complex oxide by the reaction with yttrium. The computational analyses for observing of matrix influence and oxide phase influence on strenghtening of steels were performed. These computational analyses were based on microstructural analyses of ODS steels. There was found that the oxide particles could very effectively improve strenght of steels at room temperature and especialy at high temperature. Based on corrosion tests of 14Cr ODS steel in liquid Pb and LBE enviroment were designed surface protection of ODS steel. The effectiveness of protective layer was verified by the high temperature corrosion test of PM2000 in LBE. No damage of oxide layer was observed although Pb and Bi diffused through protective layer.
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