Cast nickel-based superalloys used as structural materials for gas turbine parts need to withstand high temperatures and dynamic mechanical loads. When in contact with ambient air, the formation of protective oxide scales causes a depletion of γ’-precipitates in the surface-near region and leaves a weakened microstructure. This environmentally based degradation of the material might be accelerated under cyclic thermal exposure. In this paper, the cyclic oxidation behavior of two cast nickel-based superalloys and one single crystalline variant are investigated: C1023, CM-247 LC and M-247 SX. Exposure tests were carried out under both isothermal and cyclic conditions in air at 850 °C, 950 °C and 1050 °C for times up to 120 h to investigate the impact of thermal cycling. The differences in oxidation mechanisms are analyzed phenomenologically via light and electron microscopy and brought in correlation with the oxidation kinetics, determined based on net mass change and depletion zone growth. An assessment of the impact of precipitation loss on local mechanical strength is attempted via nano-indentation method. The found relations can be transferred onto an acceleration of crack growth under creep-fatigue and thermo-mechanical fatigue conditions.

Effects of alloying additions of Ti or Mo to a simplified chemical composition of the γ′′-Ni 3 Nb strengthened type Ni-based alloy 718 on the precipitation mode of δ-Ni 3 Nb phase were investigated to aim at designing grain boundaries using the δ phase for raising temperature capability of the γ′′ strengthened Ni-based wrought alloys. In the base alloy of Ni-22Cr-16Fe-3.5Nb, the δ phase precipitated at the grain boundaries of the matrix phase in a platelet form by continuous precipitation mode at temperatures above 1273K (1000°C) but in a lamellar morphology by discontinuous precipitation mode below that temperature. The boundary temperature where the continuous/discontinuous precipitation mode changes was raised by addition of 1 % Ti and lowered by addition of 5% Mo. The increase in the boundary temperature by Ti addition can be considered to have occurred by an increase in the solvus temperature of γ′′ phase. The decrease in the boundary temperature by Mo addition can be interpreted by the reduction of the strain energy caused by the coherent γ′′ precipitates and/or the volume change by the formation of δ phase from the γ/γ′′ phases, which may promote the continuous precipitation with respect to the discontinuous precipitation.

Ni-38Cr-3.8Al has high hardness and high corrosion resistance with good hot workability, and therefore, it has been applied on various applications. However, in order to expand further application, it is important to understand the high temperature properties. Then, this study focused on the high temperature properties such as thermal phase stability, hardness, tensile property, creep property and hot corrosion resistance. As the result of studies, we found that the thermal phase stability of (γ/α-Cr) lamellar structure and the high temperature properties were strongly influenced by the temperature. Although the high temperature properties, except for creep property, of Ni-38Cr-3.8Al were superior to those of conventional Ni-based superalloys, the properties were dramatically degraded beyond 973 K. This is because the lamellar structure begins to collapse around 973 K due to the thermal stability of the lamellar structure. The hot corrosion resistance of Ni-38Cr-3.8Al was superior to that of conventional Ni-based superalloys, however, the advantage disappeared around 1073 K. These results indicate that Ni-38Cr-3.8Al is capable as a heat resistant material which is required the hot corrosion resistance rather than a heat resistant material with high strength at high temperature.

In the present study, the Inconel 617B superalloy welded trial rotor was fabricated by narrow gap tungsten inert gas (NG-TIG) welding and the effects of temperature on fracture toughness of its welded joint were investigated at 650 ℃ and 730 ℃. Fracture toughness (J0.2) of the base metal was much higher than that of the weld metal at the same temperature, which was attributed to its excellent macroscopical plasticity and the interactions of strain localization, misorientation, and coincidence site lattice (CSL) boundaries. For the base metal, the value of J0.2 was higher at 730 ℃ than at 650 ℃, resulting from the appreciable increase in ductility and decrease in strain localization as the temperature increased. For the weld metal, higher temperature (730 ℃) reduced strength but hardly improved plasticity, and the regions of high strain localization uniformly distributed in the weld metal, resulting in completely tearing the whole interface apart and lower fracture toughness of the weld metal.

In this study, creep rupture behaviors and rupture mechanisms of dissimilar welded joint between Inconel 617B and COST E martensitic steel were investigated. Creep tests were conducted at 600 ℃ in the stress range 140-240 MPa. Scanning electron microscopy (SEM) and micro-hardness were used to examine the creep rupture behaviors and microstructure characteristics of the joint. The results indicated that the rupture positions of crept joints shifted as stress changed. At higher stress level, the rupture position was located in the base metal (BM) of COST E martensitic steel with much plastic deformation and necking. At relatively lower stress level, the rupture positions were located in the fine-grained heat affected zone (FGHAZ) of COST E or at the interface between COST E and WM both identified to be brittle fracture. Rupture in the FGHAZ was caused by type Ⅳ crack due to matrix softening and lack of sufficient precipitates pinning at the grain boundaries (GBs). Rupture at the interface was related to oxide notch forming at the interface.

It is required to reduce the lifetime cost of turbine blades. To achieve the cost reduction, a refining and recycling method of scrapped turbine blades is proposed. For the establishment of the method, desulfurization mechanism of Ni-base superalloy by solid CaO was studied. 500 g of superalloy containing sulfur was heated in a vacuum induction furnace and kept at 1600 °C. A CaO rod was inserted into the molten alloy and held for 600 s. After the experiment, sulfur content in the alloy decreased from 200 ppm to 54 ppm. On the surface of the CaO rod after the experiment, only Ca, O, Al, and S were found by EPMA analysis. Especially, Al and S were distributed at the surface and grain boundaries of the rod. By powder XRD analysis, CaO, CaS and 3CaO･Al 2 O 3 were identified as constituent phases on the rod. The desulfurization mechanism of superalloy at 1600 °C is supposed to be three steps: (1) Al and S in the alloy react with CaO to generate CaS and Al 2 O 3 , respectively. (2) Al 2 O 3 melts with CaO as liquid slag. (3) CaS is captured by the slag, therefore, sulfur is removed from the alloy.

The morphological evolution of secondary γ′ precipitates under the coarsening process was investigated for commercial wrought Ni-based superalloys, which can be classified into two processes, i.e. “localization process” and “aggregation process”. The localization process was defined as a phenomenon in which cuboidal γ′ precipitates were arranged in the <100> direction for superalloys. In contrast, the aggregation process was defined as a phenomenon in which neighboring spherical γ′ precipitates coarsen while overlapping their interfaces for superalloys. All the wrought Ni-based superalloys could be classified into the above two processes based on their volume fraction and lattice misfit. The coarsening of γ′ precipitates follow the aggregation process when the misfit is smaller than 0.05%, and it follows the localization process otherwise.

The behavior of strain-induced abnormal grain growth (AGG) in superalloy 718 has been investigated using compression testing and subsequent heat treatment below the d-phase solvus temperature of 980 °C. The nuclei of AGG grains were slightly newly recrystallized grains by a nucleation because small grains without dislocation was observed in the as- deformed microstructure. AGG was caused by the difference in intragranular misorientation (related to the stored strain energy in a grain) between dynamic recrystallized grains and deformed matrix. The initiation of AGG was retarded with decreasing plastic strain and produced microstructures consisted of larger grains having more complex morphology. It was observed that grain boundary migrated locally in the direction perpendicular to, or mainly in the direction parallel to the S3 {111} twin boundaries along with the formation of high-order twins. As a result of multiple twinning, AGG grains seemed to evolve with the growing directions changed.

Inconel 740H is one of the most promising candidate Ni-base superalloys for the main steam pipe of 700 °C advanced ultra-supercritical (A-USC) coal-fired power plants. After processing and welding in manufacturing plant in solution-annealed state, large components was commonly suggested to have an extra aging treatment at 800 °C for 16 h, in order to obtain homogeneous γ′ precipitates. In this present work, creep tests and microstructure analyses were conducted on Inconel 740H pipe specimens under two different heat treatments to verify the necessity of aging process. Here we show that aging treatment has limited effect on the creep rupture life of Inconel 740H pipe. Both in grain interiors and along grain boundaries, crept specimens under two different heat treatments have the same precipitates. But the shape and distribution of γ′ in solution annealed sample is not as regular as the aged ones. Our results provide the underlying insight that aging treatment is not so necessary for the straight pipes if the on-site condition was hard to control. But for both groups of specimens, a small amount of h particles and some banded like M 23 C 6 were emerged during creep, which would be harmful to mechanical properties for the long run.

Materials are the key to develop advanced ultra-supercritical (A-USC) steam generators. Operating at temperature up to 760°C and sustained pressure up to 4500 psi. Pressure vessel and piping materials may fail due to creep, oxidation, and erosion. Valves are particularly subjected to loss of function and leakage due to impermeant of the sealing surfaces. New materials, less susceptible to the above damage modes are needed for A-USC technology. Two Ni-based superalloys have been identified as prime candidates for valves based materials. Hardfacing is applied to sealing surfaces to protect them from wear and to reduce friction. Stellite 6 (Cobalt-based alloy) is the benchmark hardfacing owing to its anti-galling properties. However, the latest results tend to indicate that it is not suitable for high pressure application above 700°C. An alternative hardfacing will be required for A-USC. New Ni- and Co- based alloys are being developed for applications where extreme wear is combined with high temperatures and corrosive media. Their chemistry accounts for the excellent dry-running properties of these alloys and makes them very suitable for use in adhesive (metal-to- metal) wear. These new alloys have better wear, erosion, and corrosion resistance than Stellite 6 in the temperature range 800°C ~ 1000°C. As such, they have the potential to operate in A-USC. Velan recently developed an instrumented high temperature tribometer in collaboration with Polytechnique Montreal to characterize new alloys including static and dynamic coefficients of friction up to 800°C. We present herein the methodology that has been devolved to explore the effects of elevated temperature on the tribological behavior of those advanced material systems, with the goal of capturing the basis for the specification, design, fabrication, operation, and maintenance of valves for A-USC steam power plants.

The powder metallurgy (P/M) process has been applied to a high strength turbine disk alloy. It is known that P/M alloys show characteristic microstructures such as prior powder boundaries (PPB) compared to microstructures of conventional cast and wrought (CW) alloys. High temperature tensile tests were conducted on CW and P/M processed alloy720Li in order to reveal the effect of temperature and strain rate on deformation behavior and to demonstrate the effect of microstructure derived from P/M process on deformability. The fracture mode of the P/M material changed from grain interior fracture to fracture around large PPB with an increment of strain rate. In addition, samples ruptured at higher temperature showed grain boundary fracture regardless of strain rate. On the other hand, the CW material showed good deformability with chisel point fracture in the entire temperature and strain rate condition range. In the P/M material, melting of grain boundaries occurred at super solvus temperature conditions. Large PPB acts as nucleation site of voids at higher strain rate conditions. Precipitation strengthening by γ’ phase degrades deformability at sub solvus temperature conditions. However, deformability near the solvus temperature and low strain rate condition in as HIPed P/M material increased with fine grain size distribution in spite of the presence of large grains resulting from PPB.

In this work, the effects of phosphorus addition on the creep properties and microstructural changes of wrought γ’-strengthened Ni-based superalloys (Haynes 282) were investigated, focusing on the effects of carbides precipitation. In an alloy with a phosphorus content of 8 ppm, precipitation of M 23 C 6 carbides was observed in both grain boundaries and the grain interior prior to the creep tests. Grain boundary coverage by carbide increased with phosphorus content up to approximately 30 ppm. On the other hand, the amount of M 23 C 6 in the grain interior decreased with phosphorus content. The results of the creep tests revealed the relationship between the time to rupture and the grain boundary coverage by carbides. The microstructure of the crept specimens showed the existence of misorientation at the vicinity of grain boundaries without carbides, as demonstrated via electron backscattered diffraction (EBSD) analysis. These results suggest that the observed improvement in the time to rupture is due to a grain-boundary precipitation strengthening mechanism caused by grain boundary carbides and that phosphorus content affects the precipitation behavior of M 23 C 6 carbides in the grain interior and grain boundaries. These behaviors were different between alloys with the single addition of phosphorus and alloys with the multiple addition of phosphorus and niobium.

This study aims to examine the effects of grain boundary oxidation and creep on crack initiation and fracture behaviors in cold worked surface layer, under static tensile stresses in air. To determine these effects in relation to percent cold work and hardness scale, cold-rolled plates with a reduction ratios between 10% and 50% were prepared. Uniaxial constant load (UCL) tests were conducted at elevated temperature in air using smooth round bar specimen. UCL tests with a load of 0.9σy (926MPa) at 550°C show that rupture time for all cold- rolled materials were shorter than that of as-received material. From cross-sectional observation after UCL testing, surface crack at grain boundary and voids were observed in as-received material, whereas creep cracks were also observed in cold-rolled materials. This implied that crack initiation was assisted by cold working. Comparing test results with a load reduced to 0.8σy (823MPa), difference of rupture time was expected as a factor of 5 for as-received material, and measured as 2-3 for cold-rolled materials. It was suggested that cold worked layer was more sensitive to creep than base metal.

Directional coarsening of the γ' phase (rafting) in Ni-based single crystal superalloys during creep at 1273 K was simulated by the phase-field method. The inelastic strain introduced in the γ phase was assumed to be composed of plastic strain (ε p ) and creep strain (ε c ). The simulations were performed with various sets of values of material parameters and the magnitude of external tensile stress. We let a feed-forward neural network learn the simulation data in order to enable fast and exhaustive prediction of the time to rafting, t raft . From the analysis based on the trained neural network, it has been shown that t raft becomes longer with increasing magnitude of γ/γ' lattice misfit, with decreasing creep coefficient, and with increasing yield stress of the γ phase (σγ ys ). The sensitivity of t raft to σ γ ys is high when the ratio of ε p to the total inelastic strain (ε p + ε c ) is high.

The relationship between the hot workability and the precipitation morphology of γ′ phase in the Alloy U520 was examined with a focus on the presence of γ′-nodule. To change the morphology of γ’ phase, forged bars of the Alloy U520 were solution treated followed by cooling process with the cooling rates of 5~100 K/h. After the heat treatment, both γ’ phases of intragranular particle and nodule along grain boundaries were observed, and the both sizes increased by slowing down the cooling rate. That is, the area fraction of γ’-nodule increased from about 0.1 % in the sample cooled at 100 K/h to about 70 % at 5 K/h. In Gleeble tension test, the slow-cooled samples basically exhibited higher ductility than water-quenched samples below the γ′-solvus temperature. However, the ductility was maximized in the sample cooled at 20 K/h, and excessive decrease of cooling rate resulted in a drop in ductility. EBSD analysis revealed that dynamic recrystallization (DRX) was often occurred in grain interior but suppressed at γ′-nodule area, indicating that presence of γ′-nodule had a negative influence on hot workability at subsolvus temperature.

Development of the advanced USC (A-USC) boiler technology has been promoted in recent years, which targets 700°C steam condition. HR6W (Ni-23Cr-7W-Ti-Nb-25Fe) and HR35 (Ni-30Cr-6W-Ti-15Fe) have been developed for A-USC boiler tubes and pipes. The former alloy is mainly strengthened by Fe 2 W type Laves phase. The latter one employs precipitation strengthening of α-Cr phase in addition to Laves phase. Characteristic alloy design of both alloys, which does not use precipitation strengthening of γ′ phase (Ni 3 Al), leads to superior ductility and resistance to stress-relaxation cracking. Stability of creep strength and microstructure has been confirmed by long-term creep rupture tests. The 100,000h average creep rupture strength of HR6W is 85MPa at 700C. That of HR35 is 126MPa at 700°C which is comparable with conventional Alloy617. Tubes of both alloys have been evaluated by the component test in Japanese national A-USC project with γ′ hardened Alloy617 and Alloy263. Detailed creep strength, deformation behavior and microstructural evolution of these alloys are described from the viewpoint of the difference in strengthening mechanisms. Capability of these alloys for A-USC boiler materials has been demonstrated by the component test in the commercial coal fired boiler as the part of the A-USC project.

Haynes 282 is a great candidate to meet advanced ultra-super-critical (A-USC) steam conditions in modern coal-fired power plants. The standard 2-step aging treatment has been designed for optimizing microstructure therefore providing excellent mechanical properties. We studied an alternative, more economical, 1-step aging treatment and compared microstructure, tensile properties at 750˚C and deformation behavior. Moreover, three cooling rates from the solution temperature were studied to simulate large-scale components conditions. We found that as much as about 20% of fine spherical intragranular γ' particles were successfully precipitated in all cases. Their average size increased as the cooling rate decreased. All four heat-treated alloys exhibited good mechanical properties at 750˚C with a yield strength well over 620MPa. As expected, the yield strength increased and the ductility decreased as the average γ' size decreased. The alloys exhibited a mixed mode of deformation, though the dominant deformation mechanism depended on the different γ' characteristics. The major operative deformation mechanism could be well predicted by strength increment calculations based on the precipitation strengthening model. Our results suggest that wrought Haynes 282 produced by a more economical 1-step aging treatment may be a reliable candidate for high temperature applications under A-USC conditions.

In this study, fatigue crack propagation behavior at lower temperature in single crystal nickel-base superalloys was investigated experimentally and analytically. Four types of compact specimens with different combinations of crystal orientations in loading and crack propagation directions were prepared, and fatigue crack propagation tests were conducted at room temperature and 450°C. It was revealed in the experiments that the crack propagated in the shearing mode at room temperature, while the cracking mode transitioned from the opening to shearing mode at 450°C. Both the crack propagation rate and the transition behavior were strongly influenced by the crystallographic orientations. To interpret these experimental results, crystal plasticity finite element analysis was carried out, taking account some critical factors such as elastic anisotropy, crystal orientations, 3-D geometry of the crack plane and the activities of all 12 slip systems in the FCC crystal. A damage parameter based on the slip plane activities derived from the crystal plasticity analysis could successfully rationalize the effect of primary and secondary orientations on the crystallographic cracking, including the crack propagation paths and crack propagation rates under room temperature. The proposed damage parameter could also explain the transition from the opening to crystallographic cracking observed in the experiment under 450°C.

Detailed knowledge of the creep and creep crack behavior is essential for a safe operation of thick-walled components in thermal power plants. High mechanical loads and temperatures of more than 700 °C often require the application of nickel-based alloys, e.g. alloy C-263. Unfortunately, manufacturing and non-destructive evaluation (NDE) of thick-walled components (> 50 mm) made of nickel-based alloys are quite challenging. Tolerable critical flaw sizes, experimentally validated for long service durations, play an important role in the quality assurance of such components. It is commonly accepted that manufacturing parameters, e.g. heat treatment procedures, have a significant influence on creep ductility and time-dependent crack behavior. By means of adjusting the process parameters, the ductility and the creep life of notched specimen can be significantly improved in the case of alloy C-263. Essential root cause is the decoration of grain boundaries with carbides which drastically influences creep crack initiation and growth. This results in significant differences for allowable critical flaw sizes and thus, the potential use of the candidate material. On a first generation of alloy C-263 “G1”, a dense population of carbides on the grain boundaries was found, which resulted in an inadmissible creep crack behavior. The resulting critical flaw sizes were only a few tenths of a millimeter. On a second generation “G2”, the grain boundary occupation was positively influenced, so that a satisfactory creep crack behavior could be found. The critical flaw sizes are in the order of one millimeter or more. A critical or impermissible material behavior under creep conditions can be demonstrated by testing smooth and notched round specimens. For example, the first generation “G1” notched round specimens fails earlier than the smooth round specimens, indicating notch sensitivity. On the second generation “G2”, however, a notch insensitivity was found. The critical defect sizes can be determined by a method that takes into account a simultaneous examination of the crack tip situation and the ligament situation.

The Haynes 282 Ni-based superalloy (57Ni-20Cr-10Co-8.5Mo-2.1Ti-1.5Al) is a very promising candidate for the fabrication by additive manufacturing of gas turbine components of complex geometries. Alloy 282 was fabricated by electron beam melting (EBM) and exposed to two different heat treatments, (a) solution anneal (SA) at 1135°C followed by the standard 2-step aging treatment (2h at 1010°C plus 8h at 788°C) and (b) SA followed by 4h 800°C. Large elongated grains were observed for the as-fabricated and annealed EBM 282 materials, with a γ′ (Ni 3 (Al,Ti)) average size of ~100 nm and 20 nm, respectively. The as-fabricated EBM 282 alloy exhibited good ductility at 20-900°C and tensile strength slightly lower than the tensile strength of wrought 282. Annealing the alloy resulted in a moderate increase of the alloy strength at 800 and 900°C but a decrease of the alloy ductility. The creep lifetime at 800°C, 200MPa of the as-fabricated and annealed EBM 282 specimens machined along the build direction was 2 times and 1.5 times superior to the expected lifetime for wrought 282, respectively. For creep specimens machined perpendicular to the build direction, the lifetimes were ~25% lower compared to the wrought alloy. These creep results are directly related to the strong grain texture of the EBM 282 alloy and the limited impact of the initial γ′ (Ni 3 (Al,Ti)) size on alloy 282 creep properties.