Creep resistance of CMSX-3 nickel base superalloy single crystals

Creep deformation in 〈001〉 oriented nickel base superalloy single crystals has been studied in an effort to assess the factors which contribute to the overall creep resistance of superalloys with high volume fractions of γ′ phase. Detailed observations of three dimensional dislocation arrangements produced by creep have been made with the use of stereo electron microscopy. In the temperature range of 800–900°C at stresses of 552 MPa or lower, the dislocation-free γ′ precipitates are resistant to shearing by dislocations. As a result, creep deformation occurs by forced bowing of dislocations through the narrow γ matrix channels on {111} planes. At moderate levels of temperature and stress there are incubation periods in virgin crystals prior to the onset of primary creep. The incubations arise because of the difficult process of filling the initially dislocation starved material with creep dislocations from widely spaced sources. When the newly generated dislocations percolate through the cross section, incubation comes to an end and primary creep begins. In primary creep neither work hardening nor any type of recovery plays an important role. The creep rate decelerates because the favorable initial thermal misfit stresses between γ and γ′ phases are relieved by creep flow. Continued creep leads to a build-up of a three-dimensional nodal network of dislocations. This three-dimensional network fills the γ matrix channels during steady state creep and achieves a quasi-stationary structure in time. In situ annealing experiments show that static recovery is ineffective at causing rearrangements in the three-dimensional network at temperatures of 850°C or lower. The kinematical dislocation replacement processes which maintain the quasi-stationary dislocation network structures during apparent steady state creep are not understood and require further study. Because of the impenetrability of the γ′ precipitates, dislocations move through the γ matrix by forced Orowan bowing, and this accounts for a major component of the creep resistance. In addition, the frictional constraint of the coherent or semi-coherent precipitates leads to the build-up of pressure gradients in the microstructure, and this provides load carrying capacity. There is also a smaller component of solid solution strengthening. Work hardening is comparatively unimportant. Finite element analysis shows that the non-deforming precipitates are increasingly stressed as creep deformation accumulates in the matrix. In the later stages of steady state creep and during tertiary creep the stresses in the precipitates rise to high enough levels to cause shearing of the γ′ particles by dislocations entering from the γ matrix. The recovery resistance of the material is in part due to a very low effective diffusion constant and in another part due to the fact that the three-dimensional dislocation networks formed in the γ matrix serve to neutralize the misfit between the γ and γ′ phases.     

High-temperature creep-deformation behavior of the Ni-based superalloy M963

The high-temperature creep-deformation behavior of a Ni-based M963 superalloy has been investigated over a broad stress range of 80 to 600 MPa at high temperatures (800 °C to 975 °C). The detailed dislocation configurations at different creep stages are examined through transmission electron microscopy (TEM). The results show that the deformation mechanism is stress and temperature dependent and mainly consists of three dislocation-controlling mechanisms: stacking faults and dislocation-pair shearing, dislocation bowing and Orowan looping, and dislocation climb.     

Creep and Stress Relaxation Anisotropy of a Single-Crystal Superalloy

In this study, the TMF stress relaxation and creep behavior at 1023 K and 1223 K (750 °C and 950 °C) have been investigated for a Ni-based single-crystal superalloy. Specimens with three different crystal orientations along their axes were tested; 〈001〉, 〈011〉, and 〈111〉, respectively. A highly anisotropic behavior during TMF stress relaxation was found where the 〈111〉 direction significantly shows the worst properties of all directions. The TMF stress relaxation tests were performed in both tension and compression and the results indicate a clear tension/compression asymmetry for all directions where the greatest asymmetry was observed for the 〈001〉 direction at 1023 K (750 °C); here the creep rate was ten times higher in compression than tension. This study also shows that TMF cycling seems to influence the creep rate during stress relaxation temporarily, but after some time it decreases again and adapts to the pre-unloading creep rate. Creep rates from the TMF stress relaxation tests are also compared to conventional constant load creep rates and a good agreement is found.     

Microstructural Degradation and the Effects on Creep Properties of a Hot Corrosion-Resistant Single-Crystal Ni-Based Superalloy During Long-Term Thermal Exposure

In the present study, the kinetics of microstructural degradation during long-term thermal exposure (LTTE) and the effects on creep deformation mechanisms of a hot corrosion-resistant single-crystal Ni-based superalloy with a low γ′ volume fraction and γ/γ′ lattice misfit were investigated in detail. The kinetic of γ′ coarsening in the experimental alloy conforms well to the Lifshitz–Slyozov–Wagner theory during LTTE at 900 °C up to 10,000 hours. The evolution of γ/γ′ lattice misfit during the LTTE was also investigated by a first attempt. The focused research emphasized on the influences of γ/γ′ lattice misfit evolution after the LTTE on the microstructural degradation, dislocation motion, and different creep mechanisms during high-temperature low-stress creep and high-temperature high-stress creep. The results show that the decreasing of the absolute values of γ/γ′ lattice misfit and change of γ′ size and morphology after the LTTE contribute to the weakening of barrier to the dislocation cutting process into γ′ precipitates during creep and the sharp reduction of stress-rupture lifetime at 950 °C/280 MPa after 1000 hours exposure. As the applied stress decreased to 230 MPa at 950 °C, the creep mechanisms change from the dislocation cutting through γ′ precipitates at high applied stress to the dislocation glide and climb around γ′ precipitates. The dislocation glide and climb by-pass deformation mechanism were not significantly influenced by the change of γ′ precipitates morphology and magnitude of γ/γ′ mismatch within 1000 hours thermal exposure, and the minimum creep rate and creep lifetime after 1000 hours thermal exposure were similar to that of the original heat-treated samples.     

Stress Rupture Fracture Model and Microstructure Evolution for Waspaloy

Stress rupture behavior and microstructure evolution of nickel-based superalloy Waspaloy specimens from tenon teeth of an as-received 60,000-hour service-exposed gas turbine disk were studied between 923 K and 1088 K (650 °C and 815 °C) under initial applied stresses varying from 150 to 840 MPa. Good microstructure stability and performance were verified for this turbine disk prior to stress rupture testing. Microstructure instability, such as the coarsening and dissolution of γ′ precipitates at the varying test conditions, was observed to be increased with temperature and reduced stress. Little microstructure variation was observed at 923 K (650 °C). Only secondary γ′ instability occurred at 973 K (700 °C). Four fracture mechanisms were obtained. Transgranular creep fracture was exhibited up to 923 K (650 °C) and at high stress. A mixed mode of transgranular and intergranular creep fracture occurred with reduced stress as a transition to intergranular creep fracture (ICF) at low stress. ICF was dominated by grain boundary sliding at low temperature and by the nucleation and growth of grain boundary cavities due to microstructure instability at high temperature. The fracture mechanism map and microstructure-related fracture model were constructed. Residual lifetime was also evaluated by the Larson–Miller parameter method.     

Neutron Diffraction Study of Strain/Stress States and Subgrain Defects in a Creep-Deformed, Single-Crystal Superalloy

A single crystal superalloy with initial sample axis 10 deg deviated from [001] was creep deformed at 1273 K (1000 °C) 235 MPa and its triaxial strain/stress state and subgrain defects were studied by neutron diffraction. Normal internal stresses with their directions close to the loading axis and their scales smaller than those perpendicular to the axis were observed and attributed to a lattice rotation toward [001] pole. The internal stress at a level approaching to the loading stress and mostly in the state of interphase stress was induced during the first stage of creep prior to rafting and associated to lattice rotation, microstrain relaxation and line-up of misoriented γ′-precipitates. The internal stress was diminished and released at final stage of creep associated with a reduction in unit-cell volume and a transition of strain/stress state between the two phases. The observation was explained by development of dislocations and raft structure during creep.     

High-Temperature Creep Degradation of the AM1/NiAlPt/EBPVD YSZ System

The failure mechanisms of a NiAlPt/electron beam physical vapor deposition yttria-stabilized-zirconia thermal barrier coating system deposited on the AM1 single crystalline substrate have been investigated under pure creep conditions in the temperature range from 1273 K to 1373 K (1000 °C to 1100 °C) and for durations up to 1000 hours. Doubly tapered specimens were used allowing for the analysis of different stress states and different accumulated viscoplastic strains for a given creep condition. Under such experiments, two kinds of damage mechanisms were observed. Under low applied stress conditions (i.e., long creep tests), microcracking is localized in the vicinity of the thermally grown oxide (TGO). Under high applied stress conditions, an unconventional failure mechanism at the substrate/bond coat interface is observed because of large creep strains and fast creep deformation, hence leading to a limited TGO growth. This unconventional failure mechanism is observed although the interfacial bond coat/top coat TGO thickening is accelerated by the mechanical applied stress beyond a given stress threshold.     

On the creep deformation of a cast near gamma TiAl alloy Ti48Al1 Nb

The steady-state creep deformation behavior of a cast two phase gamma TiAl alloy having the composition Ti48Al1Nb (at.%) has been studied. Tension creep tests using the stress increment technique (θθ₂θ₃) were conducted over the temperature range of 704–850°C at constant initial applied stress level of 103.4–241.3 MPa. The activation energy for creep over the temperature and stress regime of this study varied 317.5 kJ/mol (137.8 MPa) up to 341.0 kJ/mol (206.8 MPa) with an average value of 326.4 kJ/mol. This is well within the range of values previously measured for gamma TiAl alloys where creep controlled by volume diffusion has been suggested as rate controlling. The stress exponents meaured were 5.0 at 704°C, 4.9 at 750°C, 4.7 at 800°C and 4.46 at 850°C. Using the activation energy of 326.4 kJ/mol, the temperature compensated steady-state creep rate was plotted against long stress with all temperatures collapsing onto a single line having a slope equal to 4.95. Using conventional creep analysis, this value of the stress exponent can be taken as suggestive of dislocation climb controlled power law creep as the operative deformation mechanism within the stress and temperature regime of the present study. The boundary separating the lamellar grains in two phase gamma TiAl alloys having the duplex microstructure may be a very important aspect of this microstructure with respect to creep deformation resistance. The interlocking γ/α₂ laths making up these boundaries are expected to be very resistant to grain boundary sliding which may contribute to creep deformation in the dislocation creep regime. Finally, some previous observations along with a comparison of the creep behavior of the Ti48Al1Nb alloy to that of a Tiz.sbnd;50.3Al binary have been discussed in terms of the pre-exponential constant A in the power law creep equation. TiAl alloys having similar stress and temperature dependencies but differing steady-state strain rates over comparable stress-temperature regimes may be rationalized on the basis of differing power law creep constants which may reflect differences in stacking fault energies.     

High-Temperature Compression Behavior of Cast and Homogenized IN939 Superalloy

Hot deformation behavior of IN-939 superalloy was investigated in this work. Hot compression experiments were performed at temperatures of 1273 K, 1323 K, 1373 K, and 1423 K (1000 °C, 1050 °C, 1100 °C, and 1150 °C) at strain rates of 0.001, 0.01, 0.1, and 1 s^?1 up to a true strain of 0.8. Then variations in stress-strain curves as well as changes in microstructures of various hot-deformed samples were studied. At 1273 K to 1323 K (1000 °C to 1050 °C), dynamic recovery (DRV), and at 1373 K to 1423 K (1100 °C to 1150 °C), dynamic recrystallization (DRX), were recognized to be the main mechanisms of the alloy softening during hot compression tests. The relationships between flow stress, strain rate, and temperature were mathematically modeled with three well-known equations, and on the basis of those equations, the activation energy of hot deformation was calculated. For improvement of the proposed models, it was necessary to conduct the investigation at two temperature ranges: 1373 K to 1423 K (1100 °C to 1150 °C), in which DRX occurred, and 1273 K to 1323 K (1000 °C to 1050 °C), where DRV as well as γ′ precipitation happened. For each of the temperature ranges, a different value for activation energy was obtained, which in conjunction with the related model, can be used for simulating the deformation behavior of the alloy.     

Microstructural Evolutions During Thermal Aging of Alloy 625: Impact of Temperature and Forming Process

The microstructural evolutions occurring upon thermal aging of alloy 625 sheets were studied in the 823 K to 1173 K (550 °C to 900 °C) temperature range and for durations up to 2000 hours. TTT diagrams of the δ and γ″ phases were established based on high-resolution scanning electron microscopy and associated quantitative image analysis approaches. The evolutions of secondary carbide volume fraction were also characterized. It was observed that the precipitation domains of the γ″ and δ phases are, respectively, 823 K to 1023 K (550 °C to 750 °C) and 923 K to 1173 K (650 °C to 900 °C) and that the γ″ coarsening follows the LSW theory once these particles have an ellipsoidal morphology. The onset of grain growth, accompanied with an increase of the texture index, was observed at a temperature as low as 1173 K (900 °C). It results from the progressive dissolution of grain boundaries’ secondary carbides (especially M₆C carbides) at this temperature, a process that favors a greater mobility of grain boundaries. It is also shown that the forming process (shear spinning), even after a relaxation heat treatment, enhances and stabilizes the precipitation of the δ phase compared to as-rolled + solution heat-treated sheets. It hence slows down the precipitation of the γ″ phase, a result that is in good agreement with a thermal aging that was performed under load (i.e., during a creep test).     

The influence of applied stress and stress sense on grain boundary precipitate morphology in a nickel-base superalloy during creep

Creep induced instability of strengthening precipitates at grain boundaries is of general concern in the applications of many high temperature alloys. Having shown that the general validity of the existing mechanism for such an instability in nickel-base superalloys may be considered suspect, this paper reports and discusses the effects of both tensile and compressive creep on γ′ grain boundary precipitate morphology in an alloy consisting of γ′ (Ni₃Al) precipitates in a γ (nickel solid solution) matrix. We find that the uniform distribution of γ′ precipitates is altered by the application of uniaxial creep stress, with the stress-induced precipitate morphology depending strongly on stress sense. Tensile creep results in the dissolution of γ′ precipitates at grain boundaries aligned more or less transverse to the stress axis, with an accompanying increase in volume fraction of γ′ precipitates at grain boundaries oriented parallel to, or almost parallel to the stress axis. In contrast, the reverse change in morphology occurs during compressive creep. The observed morphology changes and their dependence on stress sense are shown to be consistent with the flow of chromium atoms from grain boundaries that are under normal compression towards grain boundaries that are under normal tension. The results conclusively demonstrate that Herring-Nabarro type diffusion in multiphase, polycrystalline alloys can cause chemical changes in grain boundary regions which, in the extreme, result in phase changes at grain boundaries. The results and proposed mechanism are discussed in terms of the findings of other investigations.     

Creep deformation in near-γ TiAl: II. influence of carbon on creep deformation in Ti-48Al-1V-0.3C

The influence of interstitial strengthening and microstructure on creep deformation has been examined in the near-γ TiAl alloy Ti-48Al-lV-0.3C. Creep studies were conducted under constant load in air at 815 °C in the stress range of 50 to 200 MPa. Significant improvement in creep resistance was observed in this alloy compared with a similar alloy (Ti-49Al-lV) containing low levels of carbon (0.07 at. pct). The degree of strengthening resulting from the addition of carbon was found to be dependent on microstructure. At 815 °C and 150 MPa, the addition of carbon reduced the minimum creep rate by a factor of approximately 20 in the equiaxedy and duplex microstructures and by a factor of 3 in the fully lamellar microstructures. Carbide precipitation occurred in this alloy when aged in the temperature range of 700 °C to 950 °C. The addition of carbon leads to a decrease in the stress exponent from 4 to 3 in the duplex and equiaxedy microstructures and the inhibition of sub-boundary formation in the duplex microstructure. This suggests that solute/dislocation interaction mechanisms, rather than a direct effect of carbide precipitates, are responsible for the significant increase in creep resistance observed in this alloy. Brian D. Worth, formerly with the Department of Materials Science and Engineering, The University of Michigan.     

Morphological Changes and Reduction Mechanism for the Weak Reduction of the Preoxidized Panzhihua Ilmenite

Morphological changes and phase transition behaviors were investigated for the weak reduction (reduction of ferric iron-to-ferrous state) of preoxidized Panzhihua ilmenite by hydrogen at 873 K to 1073 K (600 °C to 800 °C). Ilmenite was preoxidized for 4 hours at 1023 K and 1173 K (750 °C and 900 °C), respectively, before the reduction. The results revealed that there were two competing reduction routes. At high reduction temperatures, e.g., 1023 K and 1073 K (750 °C and 800 °C), ferric irons from both hematite and pseudobrookite would combine with rutile grains as formed in the preoxidation to form homogeneous ilmenite phase with pores immingled. However, at lower reduction temperatures, e.g., 873 K (600 °C), hematite and pseudobrookite are reduced mainly through direct reduction without the participation of rutile. As a result, the as-reduced ilmenites show great differences in their phase components and microstructure, especially for the Ti species. For ilmenites preoxidized at 1023 K (750 °C), most of the Ti ions present in the needlelike rutile network, but for ilmenites preoxidized at 1173 K (900 °C), Ti distributed in both irregular rutile grains and ilmenite matrix.     

Creep Strain Modeling of 9 to 12 Pct Cr Steels Based on Microstructure Evolution

Creep deformation is simulated for 9 pct Cr steels by using the Norton equation with the addition of back stresses from dislocations and precipitates. The composite model is used to represent the heterogeneous dislocation structure found in 9 to 12 pct Cr steels. Dislocation evolution is modeled by taking capturing and annihilation of free dislocations into account. Recovery of immobile dislocations is derived from the ability of dislocation climb. In spite of the fact that the initial dislocation density is high and is reduced during creep, primary creep is successfully modeled for a P92 steel. Subgrain growth is evaluated using a model by Sandström (1977). The long time subgrain size corresponds well to a frequently used empirical relation, with subgrain size inversely proportional to the applied stress.     

Effect of Boron on the Hot Ductility Behavior of a Low Carbon Advanced Ultra-High Strength Steel (A-UHSS)

This research work studied the effect of boron additions (14, 33, 82, 126, and 214 ppm) on the hot ductility behavior of a low carbon advanced ultra-high strength steel. For this purpose, specimens were subjected to a hot tensile test at different temperatures [923 K, 973 K, 1023 K, 1073 K, 1173 K, and 1273 K (650 °C, 700 °C, 750 °C, 800 °C, 900 °C, and 1000 °C)] under a constant true strain rate of 10^?3 s^?1. The reduction of area (RA) of the tested samples until fracture was taken as a measure of the hot ductility. In general, results revealed a marked improvement in hot ductility from 82 ppm B when the stoichiometric composition for BN (0.8:1) was exceeded. By comparing the ductility curve of the steel with the highest boron content (B5, 214 ppm B) and the curve for the steel without boron (B0), the increase of hot ductility in terms of RA is over 100 pct. In contrast, the typical recovery of hot ductility at temperatures below the Ar₃, where large amounts of normal transformation ferrite usually form in the structure, was not observed in these steels. On the other hand, the fracture surfaces indicated that the fracture mode tends to be more ductile as the boron content increases. It was shown that precipitates and/or inclusions coupled with voids play a meaningful role on the crack nucleation mechanism, which in turn causes hot ductility loss. In general, results are discussed in terms of boron segregation and precipitation on austenitic grain boundaries during cooling from the austenitic range and subsequent plastic deformation.     

Dependence of Accelerated Creep Rate at 580 °C and Room Temperature Yield Stress for Two Creep Resistant Steels

Two creep resistant steels, P91 and X20, were tempered for 17520 h at 650 °C or 8760 h at 750 °C to study the growth and redistribution of carbide precipitates in martensite. On specimens annealed for a different time, yield stress at room temperature and accelerated creep rate at 580 °C were determined. With increasing yield stress in the range from 350 to 650 MPa the accelerated creep rate decreased continuously by about 2 orders of magnitude from 8·10^?7 s^?1 to 5·10^?9 s^?1. For equal yield stress, the creep rate was slightly lower for the steel P91 than for the steel X20.     

Tensile Properties and Deformation Mechanisms of Haynes 282 at Various Temperatures

The effect of temperature on the deformation mechanism and corresponding tensile properties of Haynes 282 is investigated in the temperature range from room temperature to 800 °C. It is found that below 600 °C, the yield strength remains basically unchanged with increasing temperature, while, above the temperature, a dramatic decrease in the yield strength is observed. Transmission electron microscopy observations on the slightly deformed specimens reveal that, for the experimental alloy, the plastic deformation is accomplished predominantly by pairs of a/2〈101〉 dislocation shearing through γ′ precipitates at temperatures between room temperature and 600 °C and by individual matrix dislocation bypassing γ′ precipitates above 760 °C, whereas at temperatures between the two temperatures, anti-phase boundary shearing and stacking fault shearing as well as Orowan looping operate simultaneously during the initial plastic deformation. Based on the experimental observations, it is deemed that the transitions in the deformation mechanisms account for the variation of the yield strength of the experimental alloy with temperature.     

The Role of Eta Phase Formation on the Creep Strength and Ductility of INCONEL Alloy 740 at 1023 K (750 °C)

INCONEL alloy 740 is an age-hardenable nickel-based superalloy proposed for advanced ultrasupercritical steam boiler applications operating at high stress and long times above 973 K (700 °C), where creep will be the dominate deformation mode. During high-temperature exposure, the alloy can form eta phase platelets that many have suggested may be detrimental to creep strength and ductility. In this study, creep-rupture tests were conducted on smooth and notched bars of INCONEL alloy 740 at 1023 K (750 °C) for times up to 20,000 hours. Examination of the creep-rupture life, creep ductility, failure modes, and microstructure by quantitative electron microscopy shows that a small amount of eta phase does not diminish the creep performance. Applied stress appears to have a minor effect on the precipitation of the eta phase but not its growth rate. Based on the observation that the microstructure after 20,000 hours of creep exposure has reached equilibrium in comparison to thermodynamic calculations, it is concluded that 20,000 hour creep tests are adequate for prediction of long-term creep performance.     

High-Temperature Creep and Oxidation Behavior of Mo-Si-B Alloys with High Ti Contents

Multiphase alloys in the Mo-Si-B system are potential high-temperature structural materials due to their good oxidation and creep resistance. Since they suffer from relatively high densities, the current study focuses on the influence of density-reducing Ti additions on creep and oxidation behavior at temperatures above 1273 K (1000 °C). Two alloys with compositions of Mo-12.5Si-8.5B-27.5Ti and Mo-9Si-8B-29Ti (in at. pct) were synthesized by arc melting and then homogenized by annealing in vacuum for 150 hours at 1873 K (1600 °C). Both alloys show similar creep behavior at stresses of 100 to 300 MPa and temperatures of 1473 K and 1573 K (1200 °C and 1300 °C), although they possess different intermetallic volume fractions. They exhibit superior creep resistance and lower density than a state-of-the-art Ni-base superalloy (single-crystalline CMSX-4) as well as other Mo-Si-B alloys. Solid solution strengthening due to Ti was confirmed by Vickers hardness measurements and is believed to be the reason for the significant increase in creep resistance compared to Mo-Si-B alloys without Ti, but with comparable microstructural length scales. The addition of Ti degrades oxidation resistance relative to a Mo-9Si-8B reference alloy due to the formation of a relatively porous duplex layer with titania matrix enabling easy inward diffusion of oxygen.     

Influence of Prior Fatigue Cycling on Creep Behavior of Reduced Activation Ferritic-Martensitic Steel

Creep tests were carried out at 823 K (550 °C) and 210 MPa on Reduced Activation Ferritic-Martensitic (RAFM) steel which was subjected to different extents of prior fatigue exposure at 823 K at a strain amplitude of ±0.6 pct to assess the effect of prior fatigue exposure on creep behavior. Extensive cyclic softening that characterized the fatigue damage was found to be immensely deleterious for creep strength of the tempered martensitic steel. Creep rupture life was reduced to 60 pct of that of the virgin steel when the steel was exposed to as low as 1 pct of fatigue life. However, creep life saturated after fatigue exposure of 40 pct. Increase in minimum creep rate and decrease in creep rupture ductility with a saturating trend were observed with prior fatigue exposures. To substantiate these findings, detailed transmission electron microscopy studies were carried out on the steel. With fatigue exposures, extensive recovery of martensitic-lath structure was distinctly observed which supported the cyclic softening behavior that was introduced due to prior fatigue. Consequently, prior fatigue exposures were considered responsible for decrease in creep ductility and associated reduction in the creep rupture strength.