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Electron microscopy investigation of the structure of a compact extruded from nanopowder of nickel
(2007)
Changes in the structure of single-crystal (SC) superalloy SRR99 during creep at 980 °C and 200 MPa were investigated. Geometrical parameters of the y/y'-microstructure, y/y'-misfit, stresses in the phases and local misorientation of the structure were determined at defined points of the dendritic structure by use of X-ray diffraction (XRD), wavelength dispersive X-ray spectroscopy (WDXS), scanning (SEM) and transmission (TEM) electron microscopy. Correlation of the microstructural period and local misorientation of the structure with creep strain were found.
Moiré fringes for misfit measurements at incoherent y/y'-interfaces of nickel-base superalloys
(1998)
A diffusion couple between directionally solidified nickel and the single crystal Ni-base superalloy CMSX-10 was produced by hot pressing in vacuum. The diffusion couples were heat treated at temperatures between 1050 and 1250 °C. The exposed samples were characterized by SEM/EBSD/EPMA. The interdiffusion results in dissolution of the c¢-Ni3 Al in the superalloy and in growth of nickel grains towards CMSX-10. Rapid diffusion of aluminum from the superalloy into pure nickel leads to a significant formation of pores in the superalloy. The interdiffusion processes were modelled using the finite-element simulation software DICTRA with the databases TCNi5 and MobNi2, tailored specially for Ni-base superalloys. The effect of alloying elements on the interdiffusion profiles is discussed in terms of alloy thermodynamics. The calculated element concentration profiles are in good agreement with the EPMA measurements.
The interdiffusion modeling correctly predicts the shapes of the concentration profiles, e.g. kinks on the Al and Ti profiles in the vicinity of the original interface in the joint. The calculation predicts with reasonable accuracy the extent and the location of the Kirkendall porosity.
The shape of X-ray reflections from the cuboidal γ/γ'-microstructure was investigated. The measurements were performed on the 4th generation single-crystal nickel-base superalloy TMS138. It is shown that reflections from non-cubic crystallographic planes split not only in d-scale due to the different spacing of the γ- and γ'-lattices but also in the pole figure due to the tilting of γ-lattice planes. This tilting results from the elastic distortion of the γ-lattice caused by the γ/γ'-misfit. The results obtained are discussed under the methodical aspect of misfit measurement.
Pore annihilation during hot isostatic pressing (HIP) was investigated in the single-crystal nickel-base superalloy CMSX-4 experimentally by interrupted HIP tests at 1288 °C/103 MPa. The kinetics of pore annihilation was determined by density measurement and quantitative metallography. Transmission electron microscopy of a HIPed specimen showed that the pores shrink via dislocation movement on octahedral glide planes. Theoretically pore closure under HIP condition was modelled by the finite element method using crystal plasticity and large strain theories. The modelling gives a similar kinetics of pore annihilation as observed experimentally, however somewhat higher annihilation rate.
Optical and scanning electron microscopy, as well as electron microprobe analysis and electron backscatter diffraction, have been used to study diffusion processes that occur in a diffusion pair that consistsof a single-crystal CMSX-10 nickel-base superalloy and polycrystalline nickel, at temperatures of 1050–1250°C. It has been found that, in this system, the distributions of γ-stabilizing elements (Cr, Co, W, and Re) are described by the Boltzmann solution for diffusion between two semiinfinite plates of a binary alloy. The processing of these distributions has shown that the diffusion coefficients of Cr, Co, W, and Re in the multicomponent system are close to those in binary alloys of these elements with Ni. The diffusion redistribution of the elements leads to the dissolution of the γ′ phase in the nickel-base superalloy, growth of nickel grains toward the superalloy constituent of the diffusion pair, and the formation of porosity on both sides of the migrating interface, which is determined from a crystal misorientation of the alloy single crystal and nickel grains.
The thermal stability of the microstructure of a heat-resistant cobalt alloy, which consists of a γ solid solution strengthened with γ'-phase precipitates, has been studied. The temperature behavior of the dissolution of the hardening γ' phase and the kinetics of its coarsening at 700 and 800°C have been determined. It is found that, during prolonged annealing at 800°C, the γ' → β phase transformation occurs.
A new experimental technique (repeated load annealing of flat wedge shaped specimens) was proposed for characterization of microstructural degradation under creep conditions. This technique was applied to investigate the microstructural degradation of the nickel-base superalloy CMSX-4 in a wide range of temperatures and stress levels. The results obtained allowed to describe analytically the kinetics of rafting, which is important to predict the reduction of fatigue lifetime and yield stress.