Takuya Murakoshi

Crystallinity Degradation Caused by Alloying Elements Diffusion During Creep of Ni-Base Superalloy

High temperature mechanical properties of Ni-base superalloys are improved by the fine cuboidal γ’ (Ni3Al) precipitates orderly-dispersed in the γ matrix (Ni-rich matrix) because the dispersed texture in a grain inhibits dislocation motion. However, it is well known that directional coarsening of the γ’ precipitates perpendicular to a principal stress occurs not only during creep loading but also during cyclic loading and, the formation of the raft causes the decreasing of high temperature strength drastically. Therefore, it is very important to evaluate the damage of the alloys caused by creep and fatigue loading based on the change of their micro texture. In this study, the change of crystallinity of the Ni-base superalloys (CM247LC) under creep loading was analyzed by applying Electron Back-Scattered Diffraction (EBSD) method. The image quality (IQ) value obtained from the EBSD analysis was used for the quantitative evaluation of the crystallinity in the area where an electron beam of 10 nm in diameter was irradiated. The quality of the atomic alignment of both γ’ and γ phases was found to degrade with increasing creep damage. The degradation of crystallinity suggests that the ordered L12 structure of Ni3Al became disordered and the density of dislocations and vacancies increased. However, KAM (Kernel Average Misorientation) value did not change significantly with increasing creep damage. Therefore, the dominant factor of the creep damage of this alloy is the strain-induced diffusion of elements under loading, and the decrease of the crystallinity.Copyright

Elucidation of the High Cycle Fatigue Damage Mechanism of Modified 9Cr-1Mo Steel at Elevated Temperature

Modified 9Cr-1Mo steel is one of the heat-resistant steels developed for steam generator in a FBR (Fast Breeder Reactor). When it is used in a FBR, the lifetime of the steel under HCF (High Cycle Fatigue) and V-HCF (Very-High Cycle Fatigue) caused by flow-induced vibration has to be considered for assuring its long-term reliability up to 1011 cycles. Since previous studies showed that the fatigue limit did not appear up to 108 cycles, it is necessary to investigate the fatigue strength of this alloy in cycles higher than 108 cycles. In this study, in order to clarify high cycle fatigue strength and fracture mechanism of the modified 9Cr-1Mo steel, the change of the lath martensitic strengthening structure was observed in detail on the surface of specimens fractured by rotary bending fatigue tests by using EBSD (Electron Back-Scatter Diffraction) method. The Kernel Average Misorientation (KAM) value obtained from the EBSD analysis was used for the quantitative evaluation of the change of the lath martensitic texture. It was found that the average KAM values clearly decreased on the surface areas of the fractured specimens after the application of 107-108 cycles of fatigue loading at temperatures higher than 550°C. This result indicates that degradation of the lath martensitic texture occurred around the surface of specimens tested at the temperature higher than 550°C. In order to quantitatively evaluate the decrease of its strength, a hardness test was performed at room temperature by using a nanoindentation method. It was confirmed that the surface hardness of specimens decreased drastically in the specimens fractured at temperatures higher than 550°C. From these results, it was concluded that the effective 0.2%-proof stress decreased during the fatigue tests by the degradation of the lath martensitic texture caused by the fatigue loading at elevated temperatures. Further analyses are indispensable for explicating the damage mechanism more in detail.Copyright

Degradation of the Strength of Grains and Grain Boundaries of Ni-Base Superalloy under Creep and Creep-Fatigue Loadings

The degradation process of the micro texture of Ni-base superalloys was observed under fatigue and creep-fatigue loading conditions at elevated temperatures higher than 700oC by applying electron back-scatter diffraction (EBSD) analyses. The local distribution of the crystallinity of a grain and a grain boundary was defined quantitatively by analyzing the Kikuchi pattern obtained from each electron-beam-irradiated area with a diameter of 50 nm. The calculated image quality value was used for the analysis. It was found that the crystallinity of grain boundaries degraded seriously under creep-fatigue loading conditions due to the acceleration of anisotropic strain-induced diffusion of component elements. Since the initial finely-controlled strengthened micro texture disappeared due to the anisotropic diffusion of component elements, this degradation was found to cause the drastic decrease of the strength of grains and grain boundaries and thus, lifetime of the material. The decrease of the strength of both grains and grain boundaries was measured by micro tensile test system in a scanning electron microscope by making a small sample from bulk specimen using focused ion beam. The strength of a grain and a grain boundary varied drastically depending on their crystallinity, in other words, the image quality value.

Quantitative evaluation of the quality of grains and grain boundaries in copper thin films used for 3D interconnections

The relationship of mechanical properties and micro texture of electroplated copper thin films used for 3D interconnections was investigated using a SEM, and an EBSD method. As a result, it was found that the mechanical properties changed due to the change of the average grain size and the crystallinity of grains and grain boundaries.