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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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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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