Influence of molybdenum on the creep properties of nickel-base superalloy single crystals

The influence of Mo on the creep properties of single crystals of a model nickel-base superalloy has been investigated. The Mo content was systematically varied from 9.8 to 14.6 wt pet in an alloy series based on Ni-6 wt pet Al-6 wt pet Ta. The optimum initial γ-γ′ microstructure for raft development and creep strength was produced in each alloy prior to testing. The creep lives at 982 °C and 234 MPa exhibited a steep peak as a function of Mo content, with the maximum in life occurring at about 14.0 wt pet Mo. Deviations of less than 1 wt pet Mo from the optimum composition resulted in an order of magnitude drop in properties. As the Mo content was increased from 9.8 to 14.0 wt pct, the magnitude of lattice mismatch significantly increased, which was believed to be beneficial because of stronger γ-γ′ interfaces. As the Mo content was increased further from 14.0 to 14.6 w/o, the mechanical properties degraded because of the precipitation of a deleterious third phase. The results suggest that small variations in refractory metal content and initial gg′ size can have profound effects on mechanical properties. Hence, composition ranges and microstructures for the attainment of optimum mechanical properties may be somewhat limited and require close process control.     

The influence of orientation on the stress rupture properties of nickel-base superalloy single crystals

The influence of orientation on the stress rapture properties of MAR-M247 single crystals was studied. Stress rupture tests were performed at 724 MPa and 774 °C where the effect of anisotropy is prominent. The mechanical behavior of the single crystals was rationalized on the basis of the Schmid factors for the operative slip systems and the lattice rotations which the crystals underwent during deformation. The stress rupture lives at 774 °C were found to be greatly influenced by the lattice rotations required to produce intersecting slip, because second-stage creep does not begin until after the onset of intersecting slip. Crystals which required large rotations to become oriented for intersecting slip exhibited a large primary creep strain, a large effective stress level at the onset of steady-state creep, and consequently, a short stress rupture life. Those crystals having orientations within about 25° of the [001] exhibited significantly longer lives when their orientations were closer to the [001]-[011] boundary of the stereographic triangle than to the [001]-[1l 1] boundary, because they required smaller rotations to produce intersecting slip and the onset of second-stage creep. Thus, the direction off the [001], as well as the number of degrees off the [001], has a major influence on the stress rapture lives of single crystals in this temperature regime. REBECCA A. MacKAY, formerly Graduate Assistant, Case Western Reserve University, Cleveland, OH RALPH D. MAIER, formerly Assistant Professor, Case Western Reserve University     

Environmental effects on the creep behavior of a nickel-base superalloy

Environmental effects on the 760 °C creep behavior of a nickel-base superalloy are isolated by testing at varying stress levels, in laboratory air and vacuum, specimens of different gage diameters and grain sizes, and in a few cases, different grain boundary microstructures. For all specimens receiving a standard heat treatment that results in grain boundaries free of discrete carbides, the minimum creep rate is greater in air than in vacuum for a given specimen and grain size. In contrast, for specimens aged to precipitate carbides along the grain boundaries, the creep rate is lower in air than in vacuum. The minimum creep rate and the sensitivity of this rate to applied stress also are found to be functions of grain size, specimen size, and grain boundary microstructure to extents dependent on the test environments. Rationalizations of these environmental creep behaviors are suggested in terms of the apparently competing phenomena of the relative weakening of the alloy grain boundaries in the air environment, and the alloy creep strengthening in air due to the external surface oxide scale. Formerly Graduate Research Assistant, Henry Krumb School of Mines, Columbia University     

一种镍基单晶合金的组织演化与蠕变行为

通过蠕变曲线测定及组织形貌观察,研究了一种镍基单晶合金的蠕变行为和变形特征.结果表明:单晶合金在试验的温度和应力范围内,对施加应力和温度有明显的敏感性.由所得数据测算出合金的蠕变激活能和应力指数.蠕变初期在施加温度和应力场的作用下,立方γ′相逐渐转变成与施加应力轴方向垂直的N型筏状结构.稳态蠕变期间,合金的变形机制是位错攀移越过筏状γ′相,由于高温蠕变稳态阶段形成的N型γ′相筏状组织厚度较小,位错易于攀移,因而合金具有较大的应变速率.蠕变后期,由于塑性变形,在近断口处筏形γ′相转变成与应力轴方向呈45°角的形貌,合金的变形机制是位错剪切筏状γ′相.     

The effects of environment on the elevated temperature fatigue behavior of nickel-base superalloy single crystals

The effects of air and vacuum on the fatigue behavior of a nickel-base superalloy, Mar-M200, in single crystal form were investigated. Between 800° and 1400°F fracture is entirely in the Stage I mode in air and vacuum, and fatigue life is unaffected by environment. At 1700° F in both environments, fracture is predominantly in the Stage II mode and fatigue life in air is greater than that in vacuum. At both temperatures, fatigue cracking in air is internally initiated, whereas in vacuum cracking is generally initiated at the specimen surface. Identical fatigue lives in air and in vacuum between 800° and 1400° F are attributed to the fact that internally initiated cracks in air are actually propagating in a high vacuum, surface cracking being inhibited by dynamic oxidation of emerging surface slip offsets. The subsurface portion of the Stage I fracture surface produced in air tests and all of the Stage I fracture produced in vacuum tests shows a dimpled structure, whereas the Stage I fracture surface produced while the crack propagation is in air shows a cleavage appearance. At 1700° F, bulk oxidation of surface initiated cracks interferes with the plastic blunting mechanism of Stage II crack growth normally observed at this temperature, internally initiated cracks causing ultimate failure. Shorter lives in vacuum are thought to result from enhanced Stage II surface crack propagation. Formerly with Materials Engineering and Research Laboratory, Pratt and Whitney Aircraft, Middletown, Conn.     

Effect of plastic anisotropy on the creep strength of single crystals of a nickel-based superalloy

The effect of plastic anisotropy, which is caused by the arrangement of slip systems, on the creep strength of notched specimens of Ni-based superalloy single crystals, is described. It was revealed that the creep strength of the notched specimens was affected by the crystallographic orientation, not only in the tensile direction, but also in the thickness direction. The creep strength was superior in the notched specimen with the [011] tensile and [100] plate-normal orientation, whereas the notched specimen with [011] tensile and [100] plate-normal orientation exhibited extremely poor creep strength. In the case of specimens whose tensile orientation was [011], results of the creep-rupture tests at 973 K were in agreement with the assumption of the operation of {111}〈112〉 slip systems. The creep strength in the notched specimen with [001] tensile and [100] plate-normal orientations was superior to that in the notched specimen with [001] tensile and [011] plate-normal orientations. When the tensile orientation was [001], the results of the creep-rupture tests were in agreement with the assumption of the operation of {111}〈112〉 slip systems during primary creep region and {111}〈101〉 slip systems during secondary creep region.     

Hydrogen effects in [001] oriented nickel-base superalloy single crystals

The entry and subsequent interaction of hydrogen on the mechanical properties of the single crystal nickel-base super alloy CMSX-2 has been studied. Significant amounts of hydrogen were introduced by high temperature hydrogen charging in molten salts which led to an increased lattice parameter and microhardness and to a degradation in tensile elongation to failure whose extent scales with the depth of the hydrogenated zone. In this region a fracture mode change from a {111} to a {100} type also occurred. The values of the binding energy of hydrogen to solidification voids and the effective hydrogen pressure in the voids were estimate.     

Behavior of nickel-base superalloy single crystals under thermal-mechanical fatigue

The thermal-mechanical fatigue behavior of AM1 nickel-base superalloy single crystals is studied using a cycle from 600 °C to 1100 °C. It is found to be strongly dependent on crystallo-graphic orientation, which leads to different shapes of the stress-strain hysteresis loops. The cyclic stress-strain response is influenced by variation in Young’s modulus, flow stress, and cyclic hardening with temperature for every crystallographic orientation. The thermalmechanical fatigue life is mainly spent in crack growth. Two main crack-initiation mechanisms occur, depending on the mechanical strain range. Oxidation-induced cracking is the dominant damage mechanism in the lifetime of interest for turbine blades.     

Influence of secondary precipitates and crystallographic orientation on the strength of single crystals of a Ni-based superalloy

The effect of crystallographic orientation and aging heat treatment at 850 °C on the creep rupture strength of single crystals of a nickel-based superalloy was examined at 700 °C in detail. Initial tensile orientations were selected over a wide range on the standard stereographic triangle. The {111}〈112〉-type slip systems were found to be operative during the creep deformation. The creep behavior was found to be greatly influenced by the additional aging at 850 °C for 20 hours. It was found that the effect of the aging at 850 °C was quite different between orientations favored for the slip system and those favored for the (111) slip system and that the creep deformation mechanisms of these two slip systems were different. In the orientations favored for slip systems, in the single-aged specimens, a small mean surface-to-surface spacing due to hyperfine γ′ precipitates in the matrix channel promoted the slip and the primary creep. As a result of the additional aging at 850 °C, the hyperfine γ′ precipitates were dissolved into the matrix, and the resultant large mean surface-to-surface spacing between the cuboidal precipitates inhibited extensive shearing of the γ-γ′ structure by the slip system. As a result, the creep strengths of these orientations were increased in double-aged specimens; however, the low ductility associated with the difficulty of secondary noncoplanar slip did not enlarge rupture lifetime in the double-aged [001] specimen. In the orientations favored for the (111) slip system, creep deformation occurred by twinning shear through γ and γ′ precipitates, and a distinct effect of the aging at 850 °C was not observed. In the multiple orientation of the {111} -type slip systems, i.e., the and orientations, hyperfine precipitates improved creep strength because they prevented dislocations from gliding in the matrix channel in the single-aged specimens.     

Influence of precipitate morphology on intermediate temperature creep properties of a nickel-base superalloy single crystal

The influence of γ’ precipitate morphology on the-creep behavior of the single crystal nickel-base superalloy NASAIR 100 at 760-°C was investigtated. As-heat treated crystals with cuboidal γ’ particles and crystals given an additional pre-rafting treatment to form a continuous lamellar structure were creep tested at stress levels which produced rupture lives ranging from 40 to 2500 hours. At high applied stresses, the crystals with cuboidal γ’ had both lower minimum creep rates and longer rupture lives than the crystals with lamellar γ. At lower stress levels, the initially cubic γ’ material maintained a lower crep rate, but exhibited a similar rupture life compared to the pre-rafted crystals. Examination of the microstructures which developed during creep indicated that dislocations could shear the semi-coherent γ’ rafts relatively easily compared to the coherent cuboidal γ’. In tests at lower applied stresses, slow directional coarsening of the initially cuboidal γ’ resulted in the development of a lamellar structure similar to that in the pre-rafted material, such that the rupture lives of the two materials were similar.     

On the primary creep of CMSX-4 superalloy single crystals

The effect of orientation on the primary-creep mechanism of the Ni-based single-crystal superalloy CMSX-4 is examined. Four specimens with orientations within 20 deg of the [001] axis are deformed at 750 °C and 750 MPa and show a decreasing amount of primary creep as the tensile axis approaches the [001]–[011] symmetry boundary. Of these, specimen N lies within 1 deg of [013] and shows a negligible primary creep and a very low secondary creep rate. For this specimen, direct observation in the transmission electron microscope (TEM) and analysis of the shape change show that 〈112〉{111}, stacking-fault shear, is absent. Analysis of the dislocations present in the gamma precipitates and at the γ/γ′ interface shows that the only dislocations present have the Burgers vectors a/2[101] and a/2[10-1], which cannot combine to nucleate the dislocations necessary for stacking-fault shear. Thus, it is argued that the reason for the low degree of primary creep for orientations close to the [001]–[011] symmetry boundary is not the interaction between two equally stressed 〈112〉{111} systems, but the lack of either. As the orientation moves away from the [001]–[011] boundary, the range of dislocation Burgers vectors increases and stacking-fault shear is nucleated; the amount of primary creep increases as a consequence.     

Induced creep and creep/fatigue of a nickel-base superalloy at ambient temperatures

The stress controlled fatigue of Nimonic*115, a typical γ’-strengthened nickel-base superalloy, was studied at ambient temperature, using a trapezoidal wave form at 1 Hz, with stresses chosen to produce failure in the lO⁴ to lO⁴ cycle range. In tests with maximum stress greater than the proportional limit, most of the fatigue damage occurs within the first few test cycles. Much of this strain is accumulated under static load and is therefore identified as creep strain. Transmission electron microscopy shows that these creep strains occur in slip bands which disrupt the ordered γ’ precipitates. Strain is found to follow a logarithmic time dependence, which suggests a low activation energy mechanism.     

Calculation of the internal stresses and strains in the microstructure of a single crystal nickel-base superalloy during creep

The evolution of internal stresses and strains in the microstructure of a single crystal nickel-base alloy during annealing and during creep in [001] direction has been calculated using a visco-plastic model. Two limiting conditions are considered: an “overloading” case where the internal stresses reach the critical resolved shear stress of the whole γ′ volume and an “underloading” case where the critical resolved shear stress of the γ′ precipitate is reached only at distinct areas. During creep deformation a triaxial stress state evolves in the microstructure and large pressure gradients are built up. The influence of an initial coherency misfit is shown to be negligible after short times of creep. The calculations allow the prediction of flow patterns in the microstructure, creep-induced lattice parameter changes, type and arrangement of interfacial dislocations and of the dependence of the stationary strain rate on the cube or plate morphology of the γ′ phase.     

The influence of temperature and cyclic frequency on the fatigue fracture of cube oriented nickel-base superalloy single crystals

Carbon-free single crystals of Mar-M200 were tested in pulsating tension, stress-controlled fatigue at temperatures and frequencies ranging from 1033 to 1255°K and 0.033 to 1058 Hz, respectively. The axis of loading was parallel to [001], the natural growth direction for directionally-solidified nickel-base alloys. Except for the lowest frequency at the higher temperatures where creep damage was extensive, crack initiation occurred at subsurface microporosity. Cracks initiated and propagated in the Stage I mode (crystallographic cracking on the {111} slip planes) at the lower temperatures and higher frequencies, whereas Stage (perpendicular to the principal stress axis) crack initiation and propagation was found at the higher temperatures and lower frequencies. Often a transition from Stage II to Stage I crack propagation was observed. It was established that Stage I cracking occurred under conditions of heterogeneous, planar slip and Stage II cracking under conditions of homogeneous, wavy slip. A thermally activated recovery process with an activation energy of 368 KJ/mole (88 Kcal/mole) determined the instantaneous slip character,i.e., wavy or planar, at the crack tip. In addition, it was found that an optimum frequency existed for maximizing fatigue life. At frequencies below the optimum, creep damage was detrimental, while at frequencies greater than the optimum, intense, planar slip was detrimental. The optimum frequency increased with increasing temperature.     

The influence of temperature and cyclic frequency on the fatigue fracture of cube oriented nickel-base superalloy single crystals

Carbon-free single crystals of Mar-M200 were tested in pulsating tension, stress-controlled fatigue at temperatures and frequencies ranging from 1033 to 1255°K and 0.033 to 1058 Hz, respectively. The axis of loading was parallel to [001], the natural growth direction for directionally-solidified nickel-base alloys. Except for the lowest frequency at the higher temperatures where creep damage was extensive, crack initiation occurred at subsurface microporosity. Cracks initiated and propagated in the Stage I mode (crystallographic cracking on the {111} slip planes) at the lower temperatures and higher frequencies, whereas Stage (perpendicular to the principal stress axis) crack initiation and propagation was found at the higher temperatures and lower frequencies. Often a transition from Stage II to Stage I crack propagation was observed. It was established that Stage I cracking occurred under conditions of heterogeneous, planar slip and Stage II cracking under conditions of homogeneous, wavy slip. A thermally activated recovery process with an activation energy of 368 KJ/mole (88 Kcal/mole) determined the instantaneous slip character,i.e., wavy or planar, at the crack tip. In addition, it was found that an optimum frequency existed for maximizing fatigue life. At frequencies below the optimum, creep damage was detrimental, while at frequencies greater than the optimum, intense, planar slip was detrimental. The optimum frequency increased with increasing temperature.     

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 anparticles occurs. Cellular recrystallization is observed after annealing at lower temperatures. Cellular structures induced by high diffusivity of the shot-peened alloy annealed at 1050℃ 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 yb γ' particles.     

一种单晶合金的高温蠕变行为及其变形特征

通过测定一种单晶镍基合金的高温拉伸蠕变曲线及位错运动的内摩擦应力σ0,建立了综合蠕变方程,计算出稳态蠕变期间的表观蠕变激活能及相关参数.结果表明：在蠕变期间,位错运动的内摩擦应力σ0,随外加应力的提高略有提高,随温度的升高而明显降低.蠕变后期,由于缩径使样品不同位置承受不同的有效的应力,导致筏状γ＇相具有不同的粗化特征,在近断口处,载荷的有效应力增大,使筏状γ＇相扭曲且粗化加剧.界面位错网对形变硬化和回复软化具有协调作用,并减缓位错切入γ＇相,因此有利于合金蠕变抗力的提高.     

Effect of orientation on crystallographic cracking in notched nickel-base superalloy single crystal subjected to far-field cyclic compression

The effects of crystallographic orientation on the fatigue crack initiation and growth under far-field cyclic compression are discussed in single crystals of nickel-base superalloy MAR-M200. Results indicate that cracking occurs primarily due to planar slip on the {111}-type planes. Crystallographic cracking can occur on two or more slip planes simultaneously, but through-thickness cracks are not observed. In addition, it has been shown that the threshold stress intensity for crack initiation shows a strong dependence on orientation. The threshold stress intensity for crack growth in cyclic compression is 5 to 10 times the threshold for crack growth in cyclic tension.