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Role of Plasticity in Nitinol Fatigue
Shayanfard, Pejman ; Seiner,, Hanuš (oponent) ; Dlouhý, Antonín (oponent) ; Šandera, Pavel (vedoucí práce)
This doctoral thesis deals with the analysis of the role of stress risers in NiTi elements on the local cyclic evolutions of martensitic transformation, plastic deformations, and mechanical gradients at the stress risers, under both iso-thermal cyclic loading in the superelastic regime and thermal cycling under external load in actuator regime. The methodology of investigation includes both experimental measurements and finite element simulations of notched thin NiTi superelastic/shape-memory ribbons. In the experimental part of the work, the DIC method is used to capture the spatial evolutions of strain gradients around the notch, and the X-ray microdiffraction is used to analyze the local strain fields around the notch and the plasticity induced remnant martensite at the notch-tip. Besides, the finite element results help assess the corresponding evolutions of stresses and strains, martensitic transformation, and the partitioning of total strains into elastic, plastic and residual strains around the notch. In addition, the thesis includes numerical analysis investigating the effect of the design of self-expanding NiTi stents on local cyclic evolution of martensitic transformation and its relation to fatigue performance.
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Processing of Nb-containing TiAl intermetallics and its Physical and Chemical Aspects
Barták, Tomáš ; Dlouhý, Ivo (oponent) ; Zemčík, Ladislav (oponent) ; Dlouhý, Antonín (vedoucí práce)
Presented study investigates vacuum induction re-melting of Ti-46Al-7Nb (at%) intermetallic alloy in refractory crucible based on Y2O3. A series of re-melting experiments was performed at melting temperatures 1630, 1680 and 1730 C and three ranges of melting times (5, 15 and 30 minutes). Metallographic cross-sections for each experiment were prepared to obtain the data of microstructure and phase composition evaluation using SEM and EDS. A quantitative assessment of microstructure was based on an Adaptive Contrast Control (ACC) software used to estimate a volume fraction of ceramic phase in the melt. Oxygen content in the solidified met was analyzed using Inert Gas Fusion (IGF) method. Thermodynamic calculations of possible reactions are presented regarding the activity of the individual elements of intermetallic and refractory crucible. Data presented in this work based on experimental results and thermodynamic calculation could be used like guide for further melting and optimization of the TiAlNb melting process.
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Studium funkčních vlastností tenkých vláken NiTi pro aplikace v smart strukturách a textiliích
Pilch, Jan ; Dlouhý, Antonín (oponent) ; Heczko,, Oleg (oponent) ; Pokluda, Jaroslav (vedoucí práce)
Dizertační práce je z oboru technických aplikací kovových slitin s tvarovou pamětí, jejichž jedinečné vlastnosti jsou odvozené od martenzitické fázové transformace. Konkrétně se jedná o vývoj nekonvenční metody konečné termomechanické úpravy funkčních vlastností a tvaru tenkých vláken NiTi Jouleovským ohřevem a s tím spojený základní výzkum zahrnující především termomechanické zkoušky a modelování funkčních vlastností vláken, studium martenzitických fázových transformací a deformačních procesů ve slitině NiTi a studium zotavovacích a rekrystalizační procesů v kovech při velmi rychlém ohřevu ultrakrátkými pulzy řízeného elektrického výkonu. Metoda byla v rámci práce vyvinuta a nazvána FTMT-EC. Ve srovnání s konvenčním ohřevem kovového vlákna v peci, umožňuje přesné řízení nárůstu teploty a tahového napětí v rychle ohřívaném vláknu (rychlosti ohřevu ~50 000 °C/s). Pomocí metody je možné přesně řídit velmi rychlé procesy zotavení a rekrystalizace ve vlákně a přesně nastavit požadovanou mikrostrukturu s velikostí zrna nanometrických rozměrů a od ní odvozené funkční vlastnosti vláken. Byl sestrojen prototyp zařízení pro využití metody ke kontinuální úpravě vlastností vláken SMA elektrickým proudem při převíjení z cívky na cívku. Proti v současnosti využívané konvenční úpravě vláken v odporové peci je tato úprava výrazně rychlejší, efektivnější a umožňuje připravit vlákna se zcela novými vlastnostmi. Na ochranu autorských práv k metodě byla podána mezinárodní patentová přihláška. V současnosti je metoda využívána ve výzkumu funkčních textilních materiálů pro aplikace v medicíně.
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Processing and Martensitic Transformations of NiTi-based Alloys
Kuběnová, Monika ; Kroupa, Aleš (oponent) ; Zemčík, Ladislav (oponent) ; Dlouhý, Antonín (vedoucí práce)
The thesis aims at: (i) an assessment of alloy contamination which may result from vacuum induction melting of Ni-rich NiTi-based shape memory alloys in conventional porous Y2O3 crucibles. (ii) an optimization of NiTi melting conditions with respect to the alloy purity and cost efficiency. (iii) an obtaining new differential scanning calorimetry (DSC) and 3D atom probe (AP) data on martensitic transformations and related hydrogen distributions in the Ni-rich NiTi shape memory alloys subjected to heat treatments under controlled environments with systematic variation of the hydrogen partial pressure. The following experiments were carried out: – Five different melting routes were designed and carried out in order to decrease melting temperature. – Five re-melting experiments were performed at 1500 °C with holding time 2, 10 and 20 min, and at 1550 °C and 1450 °C with 20 min holding time to examine the effect of temperature and holding time on oxygen content. – Ni-rich NiTi alloys were heat treated in Regime I (annealing) and in Regime II (annealing and aging) in either hydrogen or hydrogen-helium mixture (H2 partial pressure 20, 100, 500 and 700 mbar). Reference experiment were also performed in a pure helium atmosphere. It was found that designed melting routes lead to the lowering of maximum temperature during the induction melting cycles from 1800 to 1400 °C. Despite this significant maximum temperature drop, oxygen content of the final solidified alloy does not markedly reduce. During re-melting at 1500 °C with 2 min of holding time, the content of oxygen becomes triple the initial oxygen level and does not too differ from the re-melting experiments carried out at the same melting temperature but with 10 min of holding time. Furthermore, the oxygen content increases about fourfold with respect to the initial oxygen level during re-melting for 20 min at 1450 °C. This contamination level does not vary markedly with further rise of the melting temperature by 100 °C. Heat treatments in the controlled gaseous environments revealed that the one-step B2-B19’ martensitic transformation ceases with the increasing partial pressure of hydrogen. A pronounced drop in the DSC peak heights occurs at the hydrogen partial pressure exceeding 100 mbar. 3D AP measurements showed that there are no local variations in the Ni and Ti compositions in the sample after the Regime I heat treatment in hydrogen. Hydrogen was found to form stable interstitial solid solution in B2 NiTi. The distribution of hydrogen atoms is inhomogeneous; they organize into nano-domains with the hydrogen content exceeding locally a level of 10 at%.
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Hodnocení homogenity ingotů slitiny Ni-Ti metodou DSC
Kuběnová, Monika ; Zemčík, Ladislav (oponent) ; Dlouhý, Antonín (vedoucí práce)
Sliitny NiTi o blízkém ekviatomárním složení niklu a titianu patří do skupiny materiálů, které vykazují tvarovou paměť. Slitiny NiTi jsou velmi atraktivní funkční materiály a to nejen diky své tvarové paměti s vysokou pevností, houževnatostí, ale i svými unikátními fyzikálními vlastnostmi. Výroba těchto slitin je velmi obtížná. Striktním požadavkem na výrobu těchto slitin je dodržení chemického složení, které spolu s tepleně-mechanickými úpravami výrazně ovlivňují výsledné vlastnosti slitiny. Tato práce je zaměřena na hodnocení homogenity ingotu slitiny NiTi o nominálním složení 50,8 at.% Ni, který byl připraven vakuovým indukčním tavením v Y203 kelímku. Hodnocení homogenity se opírá zajména o metodu DSC. V práci jsou korelovány DSC výsledky s mikrostrukturou slitiny, která byla analyzována metodmami SEM a TEM.
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Role of Plasticity in Nitinol Fatigue
Shayanfard, Pejman ; Seiner,, Hanuš (oponent) ; Dlouhý, Antonín (oponent) ; Šandera, Pavel (vedoucí práce)
This doctoral thesis deals with the analysis of the role of stress risers in NiTi elements on the local cyclic evolutions of martensitic transformation, plastic deformations, and mechanical gradients at the stress risers, under both iso-thermal cyclic loading in the superelastic regime and thermal cycling under external load in actuator regime. The methodology of investigation includes both experimental measurements and finite element simulations of notched thin NiTi superelastic/shape-memory ribbons. In the experimental part of the work, the DIC method is used to capture the spatial evolutions of strain gradients around the notch, and the X-ray microdiffraction is used to analyze the local strain fields around the notch and the plasticity induced remnant martensite at the notch-tip. Besides, the finite element results help assess the corresponding evolutions of stresses and strains, martensitic transformation, and the partitioning of total strains into elastic, plastic and residual strains around the notch. In addition, the thesis includes numerical analysis investigating the effect of the design of self-expanding NiTi stents on local cyclic evolution of martensitic transformation and its relation to fatigue performance.
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METALLURGY AND PROPERTIES OF ADVANCED NiAl-Mo EUTECTICS
Barták, Tomáš ; Kuchařová, Květa ; Záležák, Tomáš ; Dlouhý, Antonín
A NiAl-Mo eutectic alloy was melt from 99,99% purity components and cast by the drop casting technique. The drop-cast ternary alloy (nominal composition of Ni-45Al-9Mo at. %), was re-melted and directionally solidified using a high temperature optical floating zone furnace. A resulting in-situ composite consists of Ni-45,2Al matrix and Mo-10Al-4Ni fibers, all in at. %. The volume fraction of 14% Mo-fibers stems from the eutectic composition. Spacing and a diameter of Mo-fibers can be controlled within certain limits using different growth rates of the crystals. Microstructural parameters of the as-cast crystals were assessed by light microscopy, scanning and transmission electron microscopy. Backscatter diffraction shows that the NiAl-matrix and the Mo-fibers are both < 001 >-oriented with respect to the axis of the cylindrical rods. Preliminary creep experiments confirmed an immense improvement of high temperature strength due to the fine distribution of Mo-fibres. The amount of strengthening in terms of minimum creep rate can be as high as 7 orders of magnitude. Post-mortem transmission electron microscopy experiments provided evidence that creep in the temperature range of 800-900 degrees C results in an extensive formation of subgrain boundaries. The strengthening effect is very likely associated with the reactions between subgrain boundaries and fine Mo-fibres.
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AGEING OF BINARY Ti-Ni ALLOY AND ITS INFLUENCE ON TRANSFORMATION CHARACTERISTICS
Szurman, I. ; Kursa, M. ; Petlák, D. ; Dlouhý, Antonín
Transformation temperatures of binary alloys from Ti-Ni system are highly sensitive to chemical composition of the alloy. This sensitivity, however, causes rather considerable complications already during process of preparation. Transformation temperatures of bays rich in Ni can be successfully modified. The key to modification of transformation temperatures lies in use of precipitation reaction of quenched over-saturated solution for influencing of composition of TiNi matrix and thus to precise control of transformation temperatures. Principle of this method consists in metastable balance between intermetallic phase TiNi and coherent precipitates Ti3Ni4. Although the precipitate Ti3Ni4 is considered to be metastable in comparison with TiNi3, it is highly stable at temperatures below 600 degrees C. During precipitation reaction Ti3Ni4 is formed and this phenomenon is connected with decrease of Ni content in TiNi matrix, which leads to increased temperatures of phase transformations TR (temperature of formation of R-phase) and Ms (temperature 'martensite start'). It is important that transformation temperature after long-term ageing is independent on chemical composition of the alloy, and it depends only on temperature of ageing as a consequence of equilibrium between these phases. This phenomenon should not occur at ageing at higher temperatures, formation of precipitate Ti3Ni4 should occur only during cooling of the sample from the temperature of ageing. The alloy Ni50.6-Ti (at. %), prepared in high-frequency induction vacuum furnace, was chosen as experimental material. Samples of the alloy were sealed into evacuated quartz glass tube and aged at constant temperature with various durations of dwell. Afterwards transformation characteristics of the samples were determined by DSC method.
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AN INTERPLAY BETWEEN HEAT TREATMENT CONDITIONS AND B2 <-> B19 ' TRANSFORMATION IN Ni-Ti SHAPE MEMORY ALLOYS
Kuběnová, Monika ; Zálešák, Jakub ; Čermák, Jiří ; Dlouhý, Antonín
This study investigates the influence of a heat treatment atmosphere on multistage martensitic transformations in a Ti-50.9at% Ni shape memory alloy. Evacuated quartz tubes were filled with hydrogen while the hydrogen partial pressure was carefully controlled in each experiment. The encapsulated specimens were subjected to heat treatments consisting of annealing and aging. After the heat treatment, the path of martensitic transformation was investigated using differential scanning calorimetry (DSC). On cooling, martensite initial temperatures decrease with the increasing partial pressure of hydrogen applied during the heat treatment. Moreover, the formation of martensite phase may not take place for partial pressures that exceed a certain limit. On the other hand, two-and multiple-step B2/R/B19' martensitic transformations are observed in specimens heat treated at lower hydrogen pressures. Results obtained using transmission electron microscopy (TEM) clearly show that the size of Ni4Ti3 precipitates becomes smaller in alloys that were heat treated at higher hydrogen pressures. The results are discussed in terms of a chain of events. It is suggested that diffusion of hydrogen into the specimen during the annealing step first influences the nucleation of the Ni4Ti3 phase. The sizes and distribution of the Ni4Ti3 precipitates than control the characteristics of B2/B19' transformation.
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Výroba, tepelné zpracování a charakterizace tenkých vrstev slitin NiTi
Svatuška, Michal ; Vokoun, David (vedoucí práce) ; Dlouhý, Antonín (oponent) ; Novák, Pavel (oponent)
Slitiny NiTi s přibližně ekviatomárním chemickým složením jsou nej- studovanější a nejvíce prakticky využívané materiály ze skupiny slitin s tvarovou pamětí (SMA). Slitina NiTi má termoelastickou martensitickou transformaci (MT), na které jsou založené její dvě nejvýznamnější vlastnosti: tvarová pamět' a su- perelasticita. Tenké filmy slitin NiTi o tloušt'kách od stovek nm po jednotky µm mají široké uplatnění hlavně v mikroelektromechanických systémech (MEMS). Dizertační práce se zabývá výrobou tenkých filmů NiTi nanášením na křemíkové substráty pomocí dvou technik - magnetronového naprašování a pulzní laserové depozice (PLD), vyšetřováním jejich mikrostruktury pomocí rentgenové difrakce, tepelným zpracováním amorfních NiTi filmů a ověřením MT pomocí rezistome- trie. Kromě toho jsou studovány termomechanické vlastnosti systému NiTi- polyimid (NiTi-PI), zejména závislost poloměru křivosti dvojvrstvy NiTi-PI na teplotě. 1
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