Solving Recent Challenges for Wrought Ni-Base Superalloys

Metallurgical and Materials Transactions A - This paper reviews the status of technology in design and manufacture of new wrought polycrystalline Ni-base superalloys for critical engineering...     

On Shear Testing of Single Crystal Ni-Base Superalloys

Shear testing can contribute to a better understanding of the plastic deformation of Ni-base superalloy single crystals. In the present study, shear testing is discussed with special emphasis placed on its strengths and weaknesses. Key mechanical and microstructural results which were obtained for the high-temperature (T?≈?1000 °C) and low-stress (τ?≈?200 MPa) creep regime are briefly reviewed. New 3D stereo STEM images of dislocation substructures which form during shear creep deformation in this regime are presented. It is then shown which new aspects need to be considered when performing double shear creep testing at lower temperatures (T?<?800 °C) and higher stresses (τ?>?600 MPa). In this creep regime, the macroscopic crystallographic [11?2](111) shear system deforms significantly faster than the [01?1](111) system. This represents direct mechanical evidence for a new planar fault nucleation scenario, which was recently suggested (Wu et al. in Acta Mater 144:642–655, 2018). The double shear creep specimen geometry inspired a micro-mechanical in-situ shear test specimen. Moreover, the in-situ SEM shear specimen can be FIB micro-machined from prior dendritic and interdendritic regions. Dendritic regions, which have a lower γ′ volume fraction, show a lower critical resolved shear stress.     

Oxidation-Assisted Crack Growth in Single-Crystal Superalloys during Fatigue with Compressive Holds

The mechanism of oxidation-assisted growth of surface cracks during fatigue with compressive holds has been studied experimentally and via a model that describes the role of oxide and substrate properties. The creep-based finite element model has been employed to examine the role of material parameters in the damage evolution in a Ni-base single-crystal superalloy René N5. Low-cycle fatigue experiments with compressive holds were conducted at 1255 K and 1366 K (982 °C and 1093 °C). Interrupted and failed specimens were characterized for crack depth and spacing, oxide thickness, and microstructural evolution. Comparison of experimental to modeled hysteresis loops indicates that transient creep drives the macroscopic stress–strain response. Crack penetration rates are strongly influenced by growth stresses in the oxide, structural evolution in the substrate, and the development of \(\gamma ^{\prime }\) denuded zones. Implications for design of alloys resistant to this mode of degradation are discussed.     

Mechanism for Formation of Surface Scale during Directional Solidification of Ni-Base Superalloys

Surface scale occurs on the external surface of directionally solidified, single-crystal turbine components. It is one of the most important casting defects because it affects the grain orientation assessment and causes incipient surface melting during heat treatment. The formation of surface scale comprises a three-stage process: (1) formation of a 0.5- to 1.5-μm Al₂O₃ layer around the external surface of liquid metal as a result of the mold/metal reaction between the liquid and the mold prime coat; (2) separation of the solidified metal from the mold wall during cooling, where the Al₂O₃ layer is stripped away from the metal surface but remains adhered to the mold; and (3) subsequent oxidation of the “bare” metal to form an oxide scale at the surface. The scale comprises a mixture of oxides. It is found that TiO₂, Cr₂O₃, and Al₂O₃ form on components cast using the 1st generation alloy, SRR99; however, in the case of castings using the 3rd-generation alloy, CMSX10N it is a predominately nickel-rich oxide (likely to be NiO). On the unscaled surface, the mold and metal are in intimate contact during casting, and subsequent cooling and the Al₂O₃ layer around the external surface prevents subsequent oxidation of the casting surface.     

Desulfurization Model Using Solid CaO in Molten Ni-Base Superalloys Containing Al

Metallurgical and Materials Transactions B - Details of the desulfurization for molten Ni-base superalloys containing Al using solid CaO have been investigated, and the formula that explains the...     

Creep Behavior and Damage of Ni-Base Superalloys PM 1000 and PM 3030

Two oxide dispersion strengthening (ODS) nickel-base superalloys, a solely dispersion-strengthened alloy (PM 1000) and an additionally γ′-strengthened alloy (PM 3030) are investigated regarding creep resistance at temperatures between 600 °C and 1000 °C. The creep strength advantage of PM 3030 over PM 1000 decreases as the temperature increases due to the thermal instability of the γ′ phase. The particle strengthening contribution in both alloys increases linearly with load. However, solid solution softening leads to an apparent drop in particle strengthening in PM 1000. Deformation concentration in slip bands is more accentuated in PM 3030-R34 due to additional γ′ strengthening combined with strongly textured coarse and elongated grain structure. Finer, equiaxed grains reduce creep strength at higher temperatures due to grain boundary deformation processes and premature pore formation, but have only minor impact at low and intermediate temperatures.     

Grain Selection During Casting Ni-Base, Single-Crystal Superalloys with Spiral Grain Selector

The behavior of grain selection in a spiral grain selector during investment casting of a Ni-base, single-crystal (SX) superalloy, DD3, has been investigated by electron backscattered diffraction (EBSD) techniques and optical microscopy. The results indicated that the main function of starter block is to optimize the crystal orientation. During the process of grain selection in spiral passage, the grain near the inner wall of spiral passage was usually selected as the final single crystal. It was found that the dendrites near the inner wall could develop new tertiary dendritic arms that paralleled the primary dendrites from the secondary dendritic arms to overgrow the dendrites far away from the inner wall. The crystal orientation that was examined by X-ray diffraction revealed that (1) the crystal orientation did not change obviously with increasing spiral thickness or angle and (2) the crystal orientation could be optimized by increasing the withdrawal rate and ceramic mold temperature. The influence of pouring temperature on crystal orientation was also discussed.     

A New Oxide Morphology Map: Initial Oxidation Behavior of Ni-Base Single-Crystal Superalloys

Predictions for oxidation behavior of Ni-base superalloys become more difficult than before because of the complex alloy composition. In this study, we focus on the initial oxidation behavior of Ni-base superalloys, and we suggest a new diagram to predict the initial oxide morphology of Ni-base superalloys with 63 binary, ternary, and multicomponent Ni-base single-crystal superalloys at 1373 K (1100 °C). As a comparison of observed and calculated weight changes after one cycle at 1373 K (1100 °C) obtained by a regression analysis, 63 alloys demonstrated two distinct behaviors, which are divided heretofore into group A and group B. Microstructural observation revealed that an oxide layer in the group A alloys consists of Al₂O₃ and/or spinel or complex oxide, whereas an oxide layer in the group B alloys consists of a thick NiO layer with an Al₂O₃ internal subscale. Thermodynamic properties can reflect more effects of alloy elements in Ni-base superalloys, and Al and Cr activities, calculated by Thermo-Calc, were used as factors to predict initial oxidation morphology. Groups A and B alloys can clearly be divided according to Al and Cr activities. This was suggested as a new diagram to predict the initial oxide morphology of Ni-base superalloys, and possibly it can apply for any generation of Ni-base superalloys.     

Quantitative Precipitate Classification and Grain Boundary Property Control in Co/Ni-Base Superalloys

A correlative approach is employed to simultaneously assess structure and chemistry of (carbide and boride) precipitates in a set of novel Co/Ni-base superalloys. Structure is derived from electron backscatter diffraction (EBSD) with pattern template matching, and chemistry obtained with energy dispersive X-ray spectroscopy (EDS). It is found that the principal carbide in these alloys is Mo and W rich with the M₆C structure. An M₂B boride also exhibiting Mo and W segregation is observed at B levels above approximately 0.085 at. pct. These phases are challenging to distinguish in an SEM with chemical information (EDS or backscatter Z-contrast) alone, without the structural information provided by EBSD. Only correlative chemical and structural fingerprinting is necessary and sufficient to fully define a phase. The identified phases are dissimilar to those predicted using ThermoCalc. We additionally perform an assessment of the grain boundary serratability in these alloys, and observe that significant amplitude is only obtained in the absence of pinning intergranular precipitates.

     

Analysis of the Chemistry of Ni-Base Turbine Disk Superalloys Using An Alloys-By-Design Modeling Approach

The chemistry of the Ni-base superalloys used for turbine disks is critiqued by making use of the recently developed Alloys-By-Design computer-based tools. Compositions within the Ni-Cr-Co-Al-Ti-Mo-W-Ta(-Zr-C-B) design space are evaluated virtually. The assessment is made on the basis of sub-models for yield strength, creep behavior, oxidation resistance, and density; microstructural factors such as $\gamma^{\prime}$ volume fraction and $\gamma^{\prime}$ solvus temperature are considered where needed. The trade-offs between the different factors are studied in a quantitative sense. Diagrams are developed for the different alloy properties to highlight the limitations and challenges that one encounters when designing new grades of alloy or when optimizing existing grades. Composition-property maps are constructed that allow for an informed approach when defining an alloy composition. Specifically, the impact of chromium, molybdenum, and tungsten additions when mechanical behavior and lifing considerations are of concern is demonstrated.     

A Microstructure-Based Time-Dependent Crack Growth Model for Life and Reliability Prediction of Turbopropulsion Systems

The objective of this investigation was to develop an innovative methodology for life and reliability prediction of hot-section components in advanced turbopropulsion systems. A set of generic microstructure-based time-dependent crack growth (TDCG) models was developed and used to assess the sources of material variability due to microstructure and material parameters such as grain size, activation energy, and crack growth threshold for TDCG. A comparison of model predictions and experimental data obtained in air and in vacuum suggests that oxidation is responsible for higher crack growth rates at high temperatures, low frequencies, and long dwell times, but oxidation can also induce higher crack growth thresholds (ΔK _th or K _th) under certain conditions. Using the enhanced risk analysis tool and material constants calibrated to IN 718 data, the effect of TDCG on the risk of fracture in turboengine components was demonstrated for a generic rotor design and a realistic mission profile using the DARWIN^® probabilistic life-prediction code. The results of this investigation confirmed that TDCG and cycle-dependent crack growth in IN 718 can be treated by a simple summation of the crack increments over a mission. For the temperatures considered, TDCG in IN 718 can be considered as a K-controlled or a diffusion-controlled oxidation-induced degradation process. This methodology provides a pathway for evaluating microstructural effects on multiple damage modes in hot-section components.     

稀土对镍基高温合金性能影响的电子理论研究

为从理论上解释稀土元素在镍基高温合金晶界区的行为本质,建立了镍基高温合金γ相大角度重位点阵晶界模型,应用Recursion方法计算了晶界偏聚稀土元素时的态密度,稀土在晶界的偏聚能以及稀土原子间的相互作用能。计算结果表明:晶界区含有稀土时,态密度双峰的高度有所降低,态密度在高能区明显上移,稀土含量越多其对晶界态密度的影响也越大;稀土原子偏聚于晶界,且主要偏聚于晶界的压缩区;稀土原子间相互排斥,因此在晶界区易形成有序相。稀土与杂质硫相互吸引,其结果是分散和固定部分杂质,改善合金高温性能。     

On the Influence of Nb/Ti Ratio on Environmentally-Assisted Crack Growth in High-Strength Nickel-Based Superalloys

The effect of Nb/Ti ratio on environmentally-assisted crack growth of three prototype Ni-based superalloys is studied. For these alloys, the yield strength is unaltered with increasing Nb/Ti ratio due to an increase in grain size. This situation has allowed the rationalization of the factors influencing damage tolerance at 700 °C. Primary intergranular cracks have been investigated using energy-dispersive X-ray spectroscopy in a scanning transmission electron microscope and the analysis of electron back-scatter diffraction patterns. Any possible detrimental effect of Nb on the observed crack tip damage due to Nb-rich oxide formation is not observed. Instead, evidence is presented to indicate that the tertiary γ′-precipitates are dissolving ahead of the crack consistent with the formation of oxides such as alumina and rutile. Our results have implications for alloy design efforts; at any given strength level, both more and less damage-tolerant variants of these alloys can be designed.     

Alloy Composition Screening for Ni-Base Turbine Disc Superalloys Using the Creep Property of Single Crystal

This paper proposes a method for alloy composition screening using the creep property of a single crystal (SC) for designing new Ni-base powder metallurgy (P/M) turbine disc superalloys. A commercial Ni-base disc alloy, U720Li®, a Ni-Co-base disc alloy, TMW-4M3, and a Ni-base conventionally cast alloy, TM-47, were selected for investigation. Their SC and P/M samples were prepared such that their γ/γ′ structures were similar. Moreover, tensile creep tests were performed on SC samples, and compressive creep tests were performed on SC and P/M samples. The tensile creep test results of SC samples at 1073 K (800 °C) and 735 MPa indicate that 0.2 and 1 pct creep times, as well as rupture life, are long in the order of TM-47 SC, TMW-4M3 SC, and U720Li SC. These results simulate the intragranular creep resistances of the corresponding P/M alloys. Furthermore, there is no significant difference in 0.2 and 1 pct compressive creep times between the SC and P/M samples of each alloy. Additionally, the 0.2 and 1 pct creep times of tensile and compressive creep tests of every alloy had an identical order. Therefore, alloy composition screening using SC creep property enables the design of new disc alloys with excellent creep resistance.

     

An Abrupt Transition to an Intergranular Failure Mode in the Near-Threshold Fatigue Crack Growth Regime in Ni-Based Superalloys

Cyclic near-threshold fatigue crack growth (FCG) behavior of two disk superalloys was evaluated and was shown to exhibit an unexpected sudden failure mode transition from a mostly transgranular failure mode at higher stress intensity factor ranges to an almost completely intergranular failure mode in the threshold regime. The change in failure modes was associated with a crossover of FCG resistance curves in which the conditions that produced higher FCG rates in the Paris regime resulted in lower FCG rates and increased ?K_th values in the threshold region. High-resolution scanning and transmission electron microscopy were used to carefully characterize the crack tips at these near-threshold conditions. Formation of stable Al-oxide followed by Cr-oxide and Ti-oxides was found to occur at the crack tip prior to formation of unstable oxides. To contrast with the threshold failure mode regime, a quantitative assessment of the role that the intergranular failure mode has on cyclic FCG behavior in the Paris regime was also performed. It was demonstrated that even a very limited intergranular failure content dominates the FCG response under mixed mode failure conditions.     

Vacuum Levels Needed to Simulate Internal Fatigue Crack Growth in Titanium Alloys and Nickel-Base Superalloys: Thermodynamic Considerations

Prior studies have examined fatigue growth of surface cracks in vacuum to simulate subsurface growth in Ti alloys and Ni-base superalloys. Even with the highest vacuum level attained using ??state-of-the-art?? pumps, it is unclear if conditions of internal crack growth are truly simulated. We consider thermodynamics of the oxidation process to help answer this question. This consideration helps explain a previously reported anomalous behavior of longer life in air than in vacuum under certain material/test conditions.     

Quenching Differential Thermal Analysis and Thermodynamic Calculation to Determine Partition Coefficients of Solute Elements in Simplified Ni-Base Superalloys

In this article, a profile-fitting methodology was developed to measure the partition coefficients of solute elements during the solidification of Ni-base alloys. Better agreement with the theoretically calculated values is expected if the accuracy of the composition and the homogeneity of the model alloys are enhanced. Regular differential thermal analysis (DTA) measurements were consistently higher than the theoretical transition temperatures, and the differences were smaller when compared to the predictions performed with the thermodynamical database developed by Du et al. The better agreement between the experimental results and the theoretical predictions made with the newly developed database suggests that improvements in the accuracy of the theoretical predictions can still be obtained and are necessary for accurate freckling prediction. Quenching modified DTA (MDTA) experiments were proven to be appropriate for directly measuring the average partition coefficients of the solute elements. Regarding the cooling rate of the first stage of the quenching experiments, it was assumed successfully that the cooling rate prior to the quenching step of 0.083 Ks⁻¹ was sufficiently slow to permit easy quenching, while being fast enough for the primary solidification reaction to depart from the equilibrium model and being closer to the Scheil model of segregation. The minimization of the error function defined from the Scheil equation was found to be an appropriate method for describing the segregation profiles of the quenched samples and permitted good estimations of the partition coefficients of the solute elements. The reliability of the methodology was found to be satisfactory given that the magnitudes calculated for the partition coefficients of the solutes in the multicomponent alloy 718 were found to be very close to the values reported in the literature.