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The creep behavior of single crystals of the nickel-based superalloy CMSX-4 was investigated at 1288 °C, which is the temperature of the hot isostatic pressing treatment applied to this superalloy in the industry. It was found that at this super-solvus temperature, where no gammaPrime-strengthening occurs, the superalloy is very soft and rapidly deforms under stresses between 4 and 16 MPa. The creep resistance was found to be very anisotropic, e.g., the creep rate of [001] crystals was about 11 times higher than that of a [111] crystal. The specimens of different orientations also showed a very different necking behavior. The reduction of the cross-sectional area psi of [001] crystals reached nearly 100 pct, while for a [111] crystal psi = 62 pct. The EBSD analysis of deformed specimens showed that despite such a large local strain the [001] crystals did not recrystallize, while a less deformed [111] crystal totally recrystallized within the necking zone. The recrystallization degree was found to be correlated with deformation behavior as well as with dwell time at high temperature. From the analysis of the obtained results (creep anisotropy, stress dependence of the creep rate, traces of shear deformation, and TEM observations), it was concluded that the main strain contribution resulted from <01-1>{111} octahedral slip.
A γ-analogue of the superalloy CMSX-4 that does not contain the strengthening γ′ -phase and only consists of the γ-solid solution of nickel has been designed, solidified as single-crystals of different orientations, and tested under creep conditions in the temperature range between 1150 and 1288 °C. The tests have revealed a very high creep anisotropy of this alloy, as was previously found for CMSX-4 at supersolvus temperature of 1288 °C. This creep anisotropy could be explained by the dominance of 〈011〉{111} octahedral slip. Furthermore, the analysis of the creep data has yielded a high value of the creep activation energy, Qc≈442 kJ/mol, which correlates with the high activation energy of Re diffusion in Ni. This supports the hypothesis that dislocation motion in the γ-matrix of Re-containing superalloys is controlled by the diffusion of the Re atoms segregating at the dislocation core. The Norton stress exponent n is close to 5, which is a typical value for pure metals and their alloys. The absence of γ′ -reprecipitation after high-temperature creep tests facilitates microstructural investigations. It has been shown by EBSD that creep deformation results in an increasing misorientation of the existing low angle boundaries. In addition, according to TEM, new low angle boundaries appear due to reactions of the a/2 〈011〉 mobile dislocations and knitting of new networks.
Using the method of directional solidification, single crystals of experimental nickel-based superalloys with negative, zero, and positive γ/γ' misfits are obtained. The γ' solvus, solidus, and liquidus temperatures of the alloys are determined, and the microstructures of the alloys after directional solidification, heat treatment, and creep tests are investigated. Creep tests are performed at temperatures of 800 and 1000°C. It is found that single crystals of the alloy with a negative γ/γ' misfit have the highest creep resistance and lifetime (the crystal lattice period of the γ' phase is smaller than that of the γ matrix).
It is shown experimentally that, during annealing and creep under low applied stresses, matrix dislocation loops frequently cross-glide. The periodic length of the zigzag dislocations deposited in the interfaces is equal to that of the γ/γ'-microstructure. Initially, the zigzag dislocations move in the (001) interface by a combination of glide and climb but then they stop near the γ'-edges and align along (100). Reactions of such dislocations lead to the formation of square interfacial networks consisting of (100) oriented edge dislocations. The complex dislocation movement is explained by the inhomogeneity of the misfit stresses between γ- and γ'-lattices. The tensile components of the stress tensor drive the dislocations through the channel, whereas the shear components near the γ'-edges cause the zigzag movement and the (100) alignment. The total effect is the most efficient relaxation of the misfit stresses. The results are relevant, especially for single-crystal superalloys of the newest generations, which have an increased γ/γ'-misfit due to the high level of refractory elements.
Constitutive modelling of creep degradation due to rafting in single-crystalline Ni-base superalloys
(2009)
A constitutive model for the mechanical behaviour of single-crystalline superalloys at high temperatures has been developed. The model relies on the slip system theory and is able to predict rafting and its influence on plastic flow. The kinetics of rafting are assumed to be driven by the reduction of the internal stresses represented by the macroscopic back-stress. The rafting effect is incorporated in the model through the dependence of the Orowan stress on the channel width. The model has been validated for the alloy CMSX-4 at 950 °C. The rafting part of the model has been calibrated by measurements of the channel widths after several levels of creep strains and for several loads.
α(1 0 0) Dislocations are observed in nickel-base superalloys after creep deformation at high temperatures and low stresses. They are formed in the γ/γ´ interfaces by a three step mechanism. First, primary dislocations with Burgers vector α/2(1 0 1) and 60° character are left behind in the interfaces when dislocation loops glide through the γ channels. The 60° dislocations move into edge orientation and react forming secondary dislocations α/2(1 1 0). In the third step, new primary dislocations are knit into the already existing meshes of primary and secondary dislocations, which results in hexagonal misfit dislocation networks consisting of secondary dislocations α/2(1 1 0) and tertiary dislocations α(1 0 0), both of edge type. This self-organisation process is explained by dislocation theory and crystallography.
Creep deformation accelerates when the α(1 0 0) interfacial dislocations enter the γ´ phase. During their climb towards the opposite interface, they attain a characteristic rectangular shape. This shape and the importance of the α(1 0 0) super dislocations for creep deformation are discussed.
Rafting during high temperature deformation in a single crystal superalloy: experiments and modeling
(2012)
Experimental characterization and mechanical modeling of creep induced rafting in superalloys
(2012)
A constitutive model has been developed for the high temperature mechanical behavior of single crystal superalloys, including rafting and its consequences. The flow stress depends on the γ channel width via the Orowan stress. An evolution equation for channel widening during high temperature straining has been derived and calibrated with measurements. Therein, rafting is assumed to be driven by the relaxation of internal stresses. The model is able to represent the mechanical softening at high stresses consecutive to rafting. The model has been applied to simulate rafting during uniaxial creep in several crystal orientations, in notched specimens as well as in cyclically loaded specimens.
Data about the creep of metals and their alloys at temperatures close to the melting point are very limited. The reason is that most engineering alloys are used at temperatures below 0.6-0.8 of their melting point, so, investigation of creep at higher temperatures has usually no practical relevance. For some special applications however it is important, in our case hot isostatic pressing (HIP) of single-crystal turbine blades cast from nickel-base superalloys. In order to remove porosity the blades are HIPed at temperatures above GammaP-solvus where superalloy has no strengthening GammaP-phase and therefore is very soft. E.g., the company Howmet Castings hips the superalloy CMSX-4 at 1288°C, which corresponds to a homologous temperature of about 0.97=1561 K/1612 K (solidus temperature). Knowledge about the creep of CMSX-4 at this temperature and understanding of the creep mechanisms are necessary to model the kinetics of pore closure during HIP.
CMSX-4 single-crystals of [001] orientation and few single-crystals of different orientations, [011], [123] and [111], were tested under creep conditions at 1288°C in the stress range between 4 and 16 MPa. At this temperature which is above the GammaP-solvus (for CMSX-4 1280°C) the superalloy has single phase structure representing the Gamma-solid solution of nickel strengthened by solute atoms. On creep curves of CMSX-4 single-crystals of different orientations measured at 1288°C/10 MPa it is seen that despite such a high homological temperature, 0.97, CMSX-4 shows very high anisotropy of creep rate. The average creep rate of [001] single-crystal in the range 0-30% strain is about 11.5 time faster than that for [111], a ratio, which is even higher than at the practically relevant temperatures 750-1100°, see e.g.. Approximation the strain rate – stress dependence by the Norton power law gave a stress exponent n of about 6 which is an indication of dislocation creep. The specimen shape after testing, analysis of traces of plastic deformation by electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) investigations indicate on dislocation slip on the octahedral system <011>{11-1}.This result however does not support the current doctrine that at high temperatures creep of metals and alloys are climb controlled. It is concluded from the obtained results that even at such a high homologous temperature, 0.97, dislocation movement by slip is more preferable than by climb if only relatively week obstacles are present like solute atoms and low angle boundaries (LABs).
It is remarkable that under used testing conditions the necking and recrystallization behavior of differently oriented single-crystals is very different. E.g., the [001] single-crystal showed very large local strain during necking, Phi=99.8%, and no recrystallization (see Fig. 3a), while the [111] single-crystal small necking, Phi=62%, accompanied by recrystallization. Such a specific deformation and recrystallization has to be undestood.
The obtained creep data of CMSX-4 was introduced in a finite element model in order to simulate pore closure during commercial HIP at a temperature of 1288°C.