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High-energy ball milling and powder metallurgy methods were used to produce a partially alloyed nickel and molybdenum of γ-Ni₃Mo composition (Ni-25at.%Mo). Milled powders were cold-compacted, sintered/solutionized at 1300°C for 100h sintering followed by quenching. Three transformation studies were performed. First, the intermetallic γ-Ni₃Mo was formed from the supersaturated solution at temperatures ranging between 600°C and 900°C for up to 100h. The 100% stable γ-Ni₃Mo phase was formed at 600°C after 100h, while aging at temperatures ranging between 650°C and 850°C for 25h was not sufficient to complete the transformation. The δ-NiMo phase was observed only at 900°C as cellular and basket strands precipitates. Second, the reversed peritectoid transformation from γ-Ni₃Mo to α-Ni and δ-NiMo was performed. Supersaturated solid solution samples were first aged at 600C for 100h followed by quenching to form the equilibrium γ-Ni₃Mo phase. After that, the samples were heat treated between 910°C and 1050°C for up to 10h followed by quenching. Regardless of heat-treatment temperature, samples heat-treated for shorter times exhibited small precipitates of δ-NiMo along and within grain boundaries of α-Ni phase, and it coarsened with time. Third, the transformation from the supersaturated solution α-Ni to the peritectoid two-phase region was performed. The samples were aged between 910°C and 1050°C for up to 10h followed by quenching. Precipitates of δ-NiMo were observed in the α-Ni matrix as small particles and then coarsened with aging time. In all three cases, hardness values increased and peaked in a way similar to that of traditional aging, except that the peak occurred much rapidly in the second and third cases. In the first case, hardness increased by about 113.6% due to the development of the new phases, while the hardness increased by 90.5% and 77.2% in the second and third cases, respectively. / Master of Science / Mechanical milling and powder processing methods were used to produce Ni-25at.%Mo alloy. Nickel and molybdenum powders were milled for 10h, pressed, and then sintered at 1300°C for 100h followed by quenching. Three different phase transformation studies were performed. The goal of the first study was to investigate the formation of γ-Ni₃Mo phase from the solid solution Ni at temperatures ranging between 600°C and 900°C followed by quenching. The 100% γ-Ni3Mo phase was formed at 600°C after 100h. In the second study, the formation of α-Ni and δ-NiMo from γ-Ni₃Mo phase was performed. The heat treatments were done between 910°C and 1050°C for up to 10h followed by quenching. The γ-Ni₃Mo phase was not stable at temperatures between 910°C and 1050°C. Small precipitates of δ-NiMo along and within grain boundaries of α-Ni phase were observed, and they coarsened with time. The third study included the formation of α-Ni and δ-NiMo from solid solution Ni. The heat treatments were performed between 910°C and 1050°C for up to 10h followed by quenching. Precipitates of δ-NiMo were observed in the α-Ni matrix. In all three cases, hardness value increased and peaked with heat treatment times as particles coarsened. In the first case, hardness increased by about 113.6% due to the development of the new phases, while the hardness increased by 90.5% and 77.2% in the second and third cases, respectively.

Doctor of Philosophy (PhD) / The evolution of atomistic-level nanostructure during the early stages of both standard, high-temperature T6 heat treatment, and low-temperature secondary ageing after interruption of the former (T6I4), has been investigated in rapid hardening Al-Cu-Mg alloys using a variety of microscopy and microanalytical techniques, including transmission electron microscopy (TEM), positron annihilation spectroscopy (PAS) and atom probe tomography (APT). In order to carry out this objective, quantitative data-analysis methods were developed with respect to new cluster-finding algorithms, specifically designed for use with three-dimensional APT data. Prior to this detailed characterisation work, the actual thermal impact from both heat treatment and quenching of small, lab-scale specimens was determined through correlation of both experimental results and calculations that modelled the heat transfer conditions using the lumped capacitance method. Subsequently, the maximum diffusion distance by random walk of the solute atoms was calculated for these periods, bearing significance on the propensity for these atoms to have the ability to cluster together, rather than segregate to the dislocation loops in the microstructure, which have a relatively larger interspacing distance. Age-hardening curves for the Al-1.1Cu-xMg (x = 0, 0.2, 0.5, 0.75, 1.0, 1.7 at.%) alloys at 150ºC show that the rapid hardening phenomenon (RHP) exists for Mg compositions ≥ 0.5Mg. Given that zone-like precipitate structures were unable to be detected by TEM or APT during the early stages of ageing at 150ºC, and that statistically significant dispersions of clusters were found in the APT data after ageing for 60 s, the RHP is attributed to these clustering reactions. Identification of clusters in the APT data has been achieved using the core-linkage algorithm and they have been found to be quite small, containing only a few atoms up to a couple of tens of atoms. The RHP is governed by some critical number density of both Mg clusters and Cu-Mg co-clusters of a critical size, whereas Cu clusters do not contribute significantly to the hardening mechanism. Significance testing indicates that Mg clusters are more significant at smaller clusters sizes and Cu-Mg co-clusters more important at larger cluster sizes. Hardness results also confirm the existence of rapid early hardening during secondary ageing at 65ºC in Al-1.1Cu-1.7Mg. The mechanism of secondary rapid hardening involves a combination of both secondary clustering from solute (mainly Mg atoms) residual in solution, and pre-existing amorphous primary clusters that have slower growth kinetics at the lower secondary ageing temperature. The latter occurs mainly by vacancy-assisted diffusion of Mg atoms as evidenced by the gradual increase of the Mg:Cu ratio of co-clusters. From an alloy design point of view it is important to fully understand the solute distribution in the microstructure to be able to subsequently optimise the configuration for enhanced material properties. The change in dispersion of solute atoms during ageing was determined by combining calculations of % vacancy-solute associations with detailed measurements of the dislocation loops to estimate the solute distribution within the microstructure. The implication of the balance of solute atoms segregated to the loops compared with that in the matrix is then discussed in the context of hardnening mechanisms.

Quaternary cubic (TixCr1 − xAl~ 0.60)1 N1 coatings with 0 &lt; x &lt; 0.33 have been grown using reactive cathodic arc evaporation. When adding Ti the hardness was retained after annealing up to 1100 °C which is a dramatic improvement compared to CrAlN coatings. The coatings showed an age hardening process caused by spinodal decomposition into coherent TiCr- and Al-rich cubic TiCrAlN domains and the formation of hexagonal AlN precipitates and cubic TiCrN domains in the vicinity of the grain boundaries. The improved hardness was attributed to the stabilization of the cubic structure suppressing the formation and growth of hexagonal AlN. Furthermore, the presence of Ti atoms generated incoherent nanometer-sized crystallites within the hexagonal AlN precipitates disrupting the hexagonal lattice during the coarsening process. The addition of Ti promoted the formation of a TiO2 layer over Al2O3 resulting in a lower oxidation resistance. However, by tuning the composition it is possible to design coatings to have both good oxidation resistance and good high temperature mechanical stability. / <p>Funding Agencies|SSF project Designed multicomponent coatings, MultiFilms||</p>

This research explores the thermal stability of ZrCrAlN material system. For this purpose fourteen different compositions of ZrCrAlN coatings were deposited onto tungsten carbide substrates by using reactive cathodic arc evaporation. These compositions were further annealed at 800oC, 900oC, 1000oC and 1100oC temperatures. EDS was employed to specify the compositions. The crystal structure of the coatings were analysed by XRD, and the hardness of these coatings was determined by Nanoindentation. The experimental findings reported a significant age hardening of Zr0.16Cr0.12Al0.72N and a delayed h-AlN formation in Zr0.07Cr0.40Al0.52N. ZrCrAlN was thus proved to be thermally stable. / Multifilms,A4:2 Growth and characterization of Multicomponent Nitrides by Magnetron Sputtering and Arc evaporation

Kyoto University (京都大学) / 0048 / 新制・課程博士 / 博士(エネルギー科学) / 甲第19093号 / エネ博第317号 / 新制||エネ||64 / 32044 / 京都大学大学院エネルギー科学研究科エネルギー変換科学専攻 / (主査)教授 木村 晃彦, 教授 星出 敏彦, 教授 今谷 勝次 / 学位規則第4条第1項該当

Doctor of Philosophy (PhD) / The evolution of atomistic-level nanostructure during the early stages of both standard, high-temperature T6 heat treatment, and low-temperature secondary ageing after interruption of the former (T6I4), has been investigated in rapid hardening Al-Cu-Mg alloys using a variety of microscopy and microanalytical techniques, including transmission electron microscopy (TEM), positron annihilation spectroscopy (PAS) and atom probe tomography (APT). In order to carry out this objective, quantitative data-analysis methods were developed with respect to new cluster-finding algorithms, specifically designed for use with three-dimensional APT data. Prior to this detailed characterisation work, the actual thermal impact from both heat treatment and quenching of small, lab-scale specimens was determined through correlation of both experimental results and calculations that modelled the heat transfer conditions using the lumped capacitance method. Subsequently, the maximum diffusion distance by random walk of the solute atoms was calculated for these periods, bearing significance on the propensity for these atoms to have the ability to cluster together, rather than segregate to the dislocation loops in the microstructure, which have a relatively larger interspacing distance. Age-hardening curves for the Al-1.1Cu-xMg (x = 0, 0.2, 0.5, 0.75, 1.0, 1.7 at.%) alloys at 150ºC show that the rapid hardening phenomenon (RHP) exists for Mg compositions ≥ 0.5Mg. Given that zone-like precipitate structures were unable to be detected by TEM or APT during the early stages of ageing at 150ºC, and that statistically significant dispersions of clusters were found in the APT data after ageing for 60 s, the RHP is attributed to these clustering reactions. Identification of clusters in the APT data has been achieved using the core-linkage algorithm and they have been found to be quite small, containing only a few atoms up to a couple of tens of atoms. The RHP is governed by some critical number density of both Mg clusters and Cu-Mg co-clusters of a critical size, whereas Cu clusters do not contribute significantly to the hardening mechanism. Significance testing indicates that Mg clusters are more significant at smaller clusters sizes and Cu-Mg co-clusters more important at larger cluster sizes. Hardness results also confirm the existence of rapid early hardening during secondary ageing at 65ºC in Al-1.1Cu-1.7Mg. The mechanism of secondary rapid hardening involves a combination of both secondary clustering from solute (mainly Mg atoms) residual in solution, and pre-existing amorphous primary clusters that have slower growth kinetics at the lower secondary ageing temperature. The latter occurs mainly by vacancy-assisted diffusion of Mg atoms as evidenced by the gradual increase of the Mg:Cu ratio of co-clusters. From an alloy design point of view it is important to fully understand the solute distribution in the microstructure to be able to subsequently optimise the configuration for enhanced material properties. The change in dispersion of solute atoms during ageing was determined by combining calculations of % vacancy-solute associations with detailed measurements of the dislocation loops to estimate the solute distribution within the microstructure. The implication of the balance of solute atoms segregated to the loops compared with that in the matrix is then discussed in the context of hardnening mechanisms.

京都大学 / 0048 / 新制・課程博士 / 博士(エネルギー科学) / 甲第19093号 / エネ博第317号 / 新制||エネ||64(附属図書館) / 32044 / 京都大学大学院エネルギー科学研究科エネルギー変換科学専攻 / (主査)教授 木村 晃彦, 教授 星出 敏彦, 教授 今谷 勝次 / 学位規則第4条第1項該当 / Doctor of Energy Science / Kyoto University / DFAM