Oxidation behavior of 4774DD1 Ni-based single-crystal superalloy at 980℃ in air

The oxidation behavior of a novel Ni-based single-crystal 4774DD1 superalloy for industrial gas turbine applications was investigated by the isothermal oxidation at 980℃ and discontinuous oxidation weight gain methods.The phase constitution and morphology of surface oxides and the characteristics of the crosssection oxide film were analyzed by XRD,SEM and EDS.Results show that the oxidation kinetics of the 4774DD1 superalloy follows the cubic law,indicating its weak oxidation resistance at this temperature.As the oxidation time increases,the composition of the oxide film evolves as following:One layer consisting of a bottom Al_(2)O_(3)sublayer and an upper(Al_(2)O_(3)+NiO)mixture sublayer after oxidized for 25 h.Then,two layers composed of an outermost small NiO discontinuous grain layer and an internal layer for 75 h.This internal layer is consisted of the bottom Al_(2)O_(3)sublayer,an intermediate narrow CrTaO_(4)sublayer,and an upper(Al_(2)O_(3)+NiO)mixture sublayer.Also two layers comprising an outermost relative continuous NiO layer with large grain size and an internal layer as the oxidation time increases to 125 h.This internal layer is composed of the upper(Al_(2)O_(3)+NiO)mixture sublayer,an intermediate continuous(CrTaO_(4)+NiWO_(4))mixture sublayer,and a bottom Al_(2)O_(3)sublayer.Finally,three layers consisting of an outermost(NiAl2O_(4)+NiCr2O_(4))mixture layer,an intermediate(CrTaO_(4)+NiWO_(4))mixture layer,and a bottom Al_(2)O_(3)layer for 200 h.

Temperature dependence of anisotropic stress-rupture properties of nickel-based single crystal superalloy SRR99

In order to reveal the temperature dependence of anisotropic stress？rupture behavior of SRR99 single crystal superalloys under conditions of temperature ranging from 650 to 1 040 °C and typical stresses,fracture morphologies and microstructure evolution were investigated by SEM and TEM.From the Larson-Miller curves,it is found that single crystal with [001] orientation has the optimum stress rupture property in comparison with [011] and [111] orientations at lower and intermediate temperature.With increasing temperature to 1 040 °C,stress-rupture properties of single crystals with three principal orientations tend to be equivalent.Based on the fracture surface and microstructural observations,superior stress？rupture behavior of single crystal with [001] orientation was rationalized and the effect of misorientation of single crystal on stress rupture property was also discussed.

Surface recrystallization of single crystal nickel-based superalloy

As-cast single crystal （SC） superalloy samples were shot peened and then annealed at different temperatures to investigate the effect of annealing temperature on the surface recrystallization behavior of the SC superalloy. The results show that the depth of recrystallized layers increases with the increase of annealing temperature. Below 1200 °C, the recrystallization depth climbs slowly with temperature rising. Above 1200 °C, the recrystallization depth increases sharply with the rise of temperature. The morphology of recrystallized grains is significantly affected by annealing temperature. Below the γ′ solvus, cellular recrystallization may be observed. Above the γ′ solvus, recrystallization occurs through the growth of well developed recrystallized grains. In addition, the microstructure evolution of recrystallized grains at the homogenization annealing temperature was studied. It is found that recrystallized grains first nucleate in the dendritic core areas on the shot-peened surface and then grow inwards along the dendritic core areas. With the dissolution of the coarse γ′ precipitates and γ/γ′ eutectics in the interdendritic areas, the recrystallized grain boundaries move through the interdendritic areas. Finally, the fully developed grains nearly have a uniform depth. The dissolution of primary γ′ precipitates is a critical factor influencing the recrystallization behavior of SC superalloys.

Microstructure evolution and deformation features of single crystal nickel-based superalloy containing 4.2% Re during creep

By means of microstructure observation and measurement of creep properties,the high temperature creep behaviors of a single crystal nickel-based superalloy containing Re were investigated.Results show that the single crystal nickel-based superalloy containing 4.2% Re possesses a better creep resistance at high temperature.After being crept up to fracture,the various morphologies are displayed in the different areas of the sample,and the γ＇ phase is transformed into the rafted structure along the direction vertical to the applied stress axis in the regions far from the fracture.But the coarsening and twisting extents of the rafted γ＇ phase increase in the regions near the fracture,which is attributed to the occurrence of the larger plastic deformation.In the later stage of creep,the deformation mechanism of the alloy is that the dislocations with [01^-1]and [011] trace features shear into the rafted γ＇ phase.The main/secondary slipping dislocations are alternately activated to twist the rafted γ＇ phase up to the occurrence of creep fracture,which is thought to be the fracture mechanism of the alloy during creep.

Effect of Ru on stress rupture properties of nickel-based single crystal superalloy at high temperature

Two experimental single crystal superalloys, Ru-free alloy and Ru-containing alloy with [001] orientation, other alloying element contents being basically kept same, were cast in the directionally solidified furnace. The effect of Ru on the stress rupture properties of the single crystal superalloy was investigated at （980 ℃, 250 MPa）, （1100 ℃, 140 MPa） and （1120 ℃, 140 MPa）. The results show that Ru can enhance high temperature stress rupture properties of single crystal superalloy. The improvement effect of Ru addition on stress rupture properties decreases with increasing test temperature. The γ′ coarsening and rafting directionally are observed in Ru-free alloy and Ru-containing alloy after stress rupture test. Needle shaped TCP phases precipitated in both of alloys after stress rupture test at （1100 ℃, 140 MPa） and （1120 ℃, 140 MPa） and no TCP phase was observed in both of alloys after stress rupture test （980 ℃, 250 MPa）. The precipitate volume fraction of TCP phases is significantly decreased by the addition of Ru. At last, the relationship between the microstructure change with Ru addition and improvement of stress rupture properties was discussed.

Creep properties and microstructure evolution of nickel-based single crystal superalloy at different conditions

The creep properties of nickel-based single crystal superalloy with [001] orientation was investigated at different test conditions. The microstructure evolution of γ′ phase, TCP phase and dislocation characteristic after creep rupture was studied by SEM and TEM. The results show that the alloy has excellent creep properties. Two different types of creep behavior can be shown in the creep curves. The primary creep is characterized by the high amplitude at test conditions of (760 °C, 600 MPa) and (850 °C, 550 MPa) and the primary creep strain is limited at (980 °C, 250 MPa), (1100 °C, 140 MPa) and (1120 °C, 120 MPa). A little change ofγ′precipitate morphology occurs at (760 °C, 600 MPa). The lateral merging of the γ′ precipitate has already begun at (850 °C, 550 MPa). Theγphase is surrounded by theγ′phase at (980 °C, 250 MPa). Theγphase is no longer continuous tested at (1070 °C, 140 MPa). At (1100 °C, 120 MPa), the thickness ofγphase continues to increase. No TCP phase precipitates in the specimens at (760 °C, 600 MPa), (850 °C, 550 MPa) and (980 °C, 250 MPa). Needle shaped TCP phase precipitates in the specimens tested at (1070 °C, 140 MPa) and (1100 °C, 120 MPa). The dislocation shear mechanism including stacking fault formation is operative at lower temperature and high stress. The dislocation by-passing mechanism occurs to form networks atγ/γ′interface under the condition of high temperature and lower stress.

Influence of Cr addition on microstructure of a 5% Re-containing single crystal nickel-based superalloy

Based on a 5% （mass fraction） Re-containing single crystal nickel-based superalloy with 3% （mass fraction） Cr, the microstructural variation with Cr addition was investigated. The experimental results show that segregation of alloying elements was enhanced in as-cast microstructure with Cr addition; and the volume fraction of eutectic is increased. However, the solidus and liquidus temperatures are remarkably reduced. With the increase of Cr content, the average γ＇ size and volume fraction are decreased in the fully heat treated microstructure. X-ray diffraction results indicate that γ/γ＇ lattice misfit becomes more negative. According to the energy dispersive spectroscopy （EDS） results, Cr is mainly distributed in the γ matrix; and more y-forming elements, such as Re and W, enter the γ matrix, while the γ/γ＇ partition ratio of Cr is inversely decreased.

Microstructual evolution and stability of second generation single crystal nickel-based superalloy DD5

The microstructual evolution and stability of a second generation single crystal (SC) nickel-based superalloy DD5 with minor grain boundary (GB) strengthening elements (C, B and Hf) were studied as a function of as-cast, heat treatment and thermal exposure. The microstructure and composition of the alloy were investigated by optical microscopy, scanning electron microanalysis (SEM), electron probe microanalysis (EPMA), energy dispersive spectrometry (EDS) and extraction analysis. In the as-cast condition,the microstructure observations and composition analysis showed that γ phase was the primary solidification phase and there were three microsegregations in the metal matrix. The morphology of these microsegregations depended on element segregations. After heat treatment, the dendrite cores contained fine and cuboidal-shaped γ′ particles with an average edge length of about 0.5 μm, whileinterdendritic regions contained irregularly-shaped γ′ particles and MC/M23C6 carbides. The mass fraction of γ′ phases was 61.685%.After exposure at 980 °C for 1000 h, no TCP phase was observed in both dendritic and interdendritic regions, indicating a good microstructual stability of the DD5 alloy at 980 °C.

Orientation dependence of transverse tensile properties of nickel-based third generation single crystal superalloy DD9 from 760 to 1100 ℃

At temperatures ranging from 760 to 1100 °C, the tensile properties of a nickel-based third generation single crystal superalloy DD9 with [100],[120] and [110] orientations were studied. The microstructures and fracture surfaces were observed by OM, SEM and TEM. Results show that the tensile strength of [100] specimen is higher than that of [120] and [110] specimens at 760 and 850 °C;while at the temperatures higher than 980 °C, the tensile strength of all specimens has little difference. The fracture mechanisms of [100],[120] and [110] specimens are the same at 760 and 980 °C. At 1100 °C, the fracture surfaces of [100] and [120] specimens are characterized by dimple features;while [110] specimen shows mixed quasi-cleavage and dimple featured fracture surfaces. At 760 °C, obvious superlattice stacking faults (SSFs) are observed only in [100] specimen;while at 1100 °C, the dislocation configurations of all specimens are similar. The difference in the number of potential active slip systems in [100],[120] and [110] specimens during the tensile deformation process is the main reason for the transverse tensile anisotropy.

Creep feed grinding induced gradient microstructures in the superficial layer of turbine blade root of single crystal nickel-based superalloy

The service performance of the turbine blade root of an aero-engine depends on the microstructures in its superficial layer.This work investigated the surface deformation structures of turbine blade root of single crystal nickel-based superalloy produced under different creep feed grinding conditions.Gradient microstructures in the superficial layer were clarified and composed of a severely deformed layer(DFL)with nano-sized grains(48–67 nm)at the topmost surface,a DFL with submicron-sized grains(66–158 nm)and micron-sized laminated structures at the subsurface,and a dislocation accumulated layer extending to the bulk material.The formation of such gradient microstructures was found to be related to the graded variations in the plastic strain and strain rate induced in the creep feed grinding process,which were as high as 6.67 and 8.17×10^(7)s^(−1),respectively.In the current study,the evolution of surface gradient microstructures was essentially a transition process from a coarse single crystal to nano-sized grains and,simultaneously,from one orientation of a single crystal to random orientations of polycrystals,during which the dislocation slips dominated the creep feed grinding induced microstructure deformation of single crystal nickel-based superalloy.

TEMPERATURE EFFECT ON LOW-CYCLE FATIGUE BEHAVIOR OF NICKEL-BASED SINGLE CRYSTALLINE SUPERALLOY

The low-cycle fatigue （LCF） behavior of a nickel-based single crystal superalloy with [001] orientation was studied at an intermediate temperature of T0℃ and a higher temperature of To ＋ 250℃ under a constant low strain rate of 10^-3 s^-1 in ambient atmosphere. The superalloy exhibited cyclic tension-compression asymmetry which is dependent on the temperature and applied strain amplitude. Analysis on the fracture surfaces showed that the surface and subsurface casting micropores were the major crack initiation sites. Interior Ta-rich carbides were frequently observed in all specimens. Two distinct types of fracture were suggested by fractogaphy. One type was characterized by Mode-I cracking with a microscopically rough surface at To ＋ 250℃. Whereas the other type at lower temperature T0℃ favored either one or several of the octahedral {111} planes, in contrast to the normal Mode-I growth mode typically observed at low loading frequencies （several Hz）. The failure mechanisms for two cracking modes are shearing of γ＇ precipitates together with the matrix at T0℃ and cracking confined in the matrix and the γ/γ＇interface at To - 250℃.

SOLIDIFICATION OF NICKEL-BASED SINGLE CRYSTAL SUPERALLOY BY ELECTRIC FIELD

The crystal growth of a nickel-based single crystal superalloy DD3 was researched via controlled directional solidification under the action of a DC electric field. The cellular or dendrite spacing of the single crystal superalloy is refined and microsegregation of alloying elements Al, Ti, Mo and W, is reduced by the electric field. The electric field decreases the interface stability and reduces the critical growth rate of the ceUular-dendritic translation because of Thomson effect and Joule heating. The precipitation of the γ＇ phase is more uniform and the size of the γ＇ phase is smaller with the electric field than that without the electric field.

Evolution mechanism of recrystallization in a nickel-based single crystal superalloy under various cooling rates during heat treatment

The recrystallization behaviors of a nickel-based single crystal superalloy during heat treatment at 1,200℃ for 4 h with various cooling rates were studied.Results show that the thickness of recrystallization layer decreases with the increase of cooling rate.In addition,the microstructures ofγ′phase in the recrystallization region are different in various cooling rates.In the high cooling rates(70,100℃·min^(-1)),small size and high volume fraction ofγ′phases are formed in the recrystallization region.It is also found that irregular fine secondaryγ′phases are precipitated between matrix channels with an average size of 150 nm in the original matric(100℃·min^(-1)).The sizes of the secondaryγ′phase decrease with the increase of cooling rate.In contrast,large size and small volume fraction ofγ′phases are formed in the recrystallization region,and a grain boundary layer is formed under a low cooling rate(10℃·min^(-1)).The evolution mechanism of recrystallization at various cooling rates during heat treatment is analyzed.

Influence of Pre-Compressive Creep on Internal Friction Stress and Creep Parameters of Nickel-Base Single Crystal Superalloys

By means of pre-compressive creep treatment, the cubic γ′ phase in a nickel base single crystal superalloy is transformed into the P-type rafted structure. And the influence of the pre-compressive creep on the internal friction stress and creep lifetimes of the superalloy are investigated by means of the measurement of the creep curves and microstructure observation. Results show that, compared to the P-type structure alloy, the full heat treated state alloy displays a bigger internal friction stress value of dislocation motion during steady state creep and a longer creep lifetimes. The creep activation energies of the full heat treated and P-type structures alloys are measured to be 462 kJ/mol and 412 kJ/mol, respectively. Thereinto, the P-type rafted γ′ phase in the alloy is transformed into the N-type structure during tensile creep. And the N-type γ′ phase transformed from the P-type structure displays a shorter size in length, this is a main reason of the P-type structure alloy possessing a shorter creep lifetimes due to creep dislocation moving easily over the rafted γ′ phase.

NUMERICAL STUDY OF THE NOTCH EFFECT ON THE CREEP BEHAVIOR AND LIFE OF NICKEL-BASE SINGLE CRYSTAL SUPERALLOYS

Numerical calculations of creep damage development and life behavior of circular notched specimens of nickel-base single crystal had been performed. The creep stress distributions depend on the specimen geometry. For a small notch radius, von Mises stress has an especial distribution. The damage distribution is greatly influenced by the notch depth, notch radius as well as notch type. The creep crack initiation place is different for each notched specimen. The characteristics of notch strengthening and notch weakening depend on the notch radius and notch type. For the same notch type, the creep rupture lives decrease with the decreasing of notch radius. A creep life model has been presented for the multiaxial stress states based on the crystallographic slip system theory.

Effect of ruthenium on γ' precipitation behavior and evolution in single crystal superalloys

The effect of Ru on γ＇ precipitation behavior and evolution in single crystal superalloys with different Ru contents were investigated by scanning electron microscopy with energy dispersive spectroscopy,3D atomic probing,differential scanning calorimetry.The results show that the solvus of the γ＇ phase decreases gradually with increasing Ru content in the alloys by casting or by the same solution and aging treatments,the alloy with a larger Ru content yields a smaller γ＇ phase.The addition of Ru increases the growth rate and coarsening rate of the γ＇ phase.Ru mainly distributes in the γ phase,which causes more Re and Mo partition into the γ＇ phase,increasing the absolute value of mismatch and the rafting rate of the γ＇ phase.

Effect of competitive crystal growth on microstructural characteristics of directionally solidified nickel-based single crystal superalloy

Directionally solidified single crystal superalloy test bars were prepared by the spiral grain selection method.The microstructural evolution and orientation characteristics of the starter block and spiral part were studied,and the influence of the competitive growth of crystals on the microstructural characteristics was analyzed.The results show that the divergent grain groups,with small size and randomly oriented grains,appear at the bottom of the start block due to the chilling effect,which is an important area for competitive growth.As the height of the starter block increases,the primary dendrite spacing increases,and the grain density decreases;furthermore,the proportion of grains with an orientation deflection angle less than 10°gradually increases.The<001>texture gradually becomes stronger as the height of the starter block increases,which indicates that the competitive growth of crystals gradually weakens.At the initial stage of the crystal selection in the spiral part,the obstacle of adjacent grains and spiral passage is the main working mechanism.The grains located at the inner side of the front edge of the spiral passage have the growth advantage.The single crystal screening process is achieved at about two-thirds of the spiral height,and the single crystal with the orientation deviation angle of 6.7°from the casting axis is prepared.

Surface recrystallization of a single crystal nickel-base superalloy

The recrystallization behavior of a single crystal nickel-base superalloy was investigated by shot peening and subsequent annealing. Two kinds of recrystallization microstructures, which are intensively dependent on the annealing temperature, are shown in the nickel-base superalloy after shot peening and subsequent annealing. Surface recrystallized grains are obtained when the superalloy is annealed at solution treatment temperature. The nucleation of recrystallization originates from the dendritic core, where rapid dissolution of γ＇ particles occurs. Cellular recrystallization is observed after annealing at lower temperatures. Cellular structures induced by high diffusivity of the moving boundary and more γ＇ particles dissolution led by residual stress are developed from the surface region. Recrystallized kinetics of the shot-peened alloy annealed at 1050°C accords with the Johnson-Mehl-Avrami-Kolmogorov equation. The low Avrami exponent is caused by the inhomogeneous distribution of stored energy, the decreasing of stored energy during recovery, and the strong resistance of boundary migration by γ＇ particles.

RAFTING PREDICTION CRITERION FOR NICKEL-BASE SINGLE CRYSTALS UNDER MULTIAXIAL STRESSES AND CRYSTALLOGRAPHIC ORIENTATION DEPENDENCE OF CREEP BEHAVIOR

Based on the relief of interfacial energy density by dislocation generation at the gamma - gamma ' interfaces, a rafting prediction criterion has been developed for nickel-base single crystals under multiaxial stresses. The diagrams of rafting have been presented, and confirmed by experimental results. The rafting process have been analyzed quantitatively by the relief of interfacial energy. The criterion has been applied to study the creep behavior. The example of creep life analysis shows that the criterion can be correlated greatly to the crystallographic orientation dependence of creep behavior. (Author abstract) 11 Refs.

Effects of directional solidification parameters and crystal selector on microstructure of single crystal of Ni-base superalloys

The single crystal of nickel-base super alloy is widely used for making turbine blades.The microstructure of the alloy,especially the deviation of preferred orientation of single crystal,possesses the most important effects on the mechanical properties of the blades.In this study,the single crystal ingot and blade of DZ417G alloy are prepared by means of the spiral crystal selector as well as the directional solidification method,and the effect of the parameters(i.e.,the shape of samples,the withdrawal rate)and the structure of the spiral crystal selector on the formation of single crystal and the crystal orientation are investigated.This method can prepare not only the single crystal ingot with simple shape but also the single crystal blades with the complex shape,the simple with rod-shape can form the single crystal easily with a relatively fast withdrawal rate,but the blade with complex shape requires much slower withdrawal rate to form single crystal.The length of the crystal selector almost has no effect on the crystal orientation.However,the angle of selector plays an obvious role on the orientation;the selector with a smaller angle can effectively reduce the deviation of preferred orientation;the appropriate angle of selector to obtain optimal orientation is found to be around30°and the deviation of preferred orientation is about30°for this selector.