Comparison of Thermodynamic Predictions and Experimental Observations on B Additions in Powder-Processed Ni-Based Superalloys Containing Elevated Concentrations of Nb

Boron additions to Ni-based superalloys are considered to be beneficial to the creep properties of the alloy, as boron has often been reported to increase grain boundary cohesion, increase ductility, and promote the formation of stable boride phases. Despite the importance, it is not well understood whether these improvements are associated with the presence of elemental boron or stable borides along the grain boundaries. In this investigation, two experimental powder-processed Ni-based superalloys containing elevated levels of Nb were found to exhibit increased solubility for B in the γ matrix when compared to similar commercial Ni-based superalloys. This resulted in an overall lower B concentration at grain boundaries that suppressed boride formation. As the predictive capability of CALPHAD database models for Ni-based superalloys have improved over the years, some discrepancies may still persist around compositionally heterogeneous features such as grain boundaries. Improved quantification of the characteristic partitioning of B as a function of the bulk alloy composition is required for understanding and predicting the stability of borides.     

Assessment of service induced microstructural damage and its rejuvenation in turbine blades

Correlations between service induced microstructural degradation and creep properties in investment cast IN738LC turbine blades are discussed. Microstructural degradation in the form of γ’ coarsen-ing, MC carbide degeneration, formation of continuous networks of grain boundary M₂₃C₆ carbides, and the disappearance of serrated grain boundaries are considered in some detail. Their influence on primary (t _p ,ε _p ), secondary (t _s , ε _s ,ε _m ) and tertiary (t_t, ε_t) creep behavior is analyzed through rela-tionships of the form:

Grain growth in dispersion strengthened superalloys by moving zone heat treatments

The high temperature strength of dispersion strengthened materials is limited by grain boundary sliding and transverse boundary rupture. These effects are minimized through development of materials with elongated or fibrous grain structures. Thermomechanical processing and grain growth heat treatments are used to develop coarse elongated grain structures in dispersion strengthened nickel-base superalloys made from mechanically alloyed powder. Grain size and aspect ratio are increased by using a moving hot zone to accomplish grain growth. The application of this technique to extruded bar of two nickel-base superalloys, IN-853* (Alloy A) and a developmental alloy (Alloy B) with composition: 15Cr, 4.5A1, 2.5Ti, 2Ta, 3.5Mo, 4W, 0.l5Zr, 0.01B, 1.1Y₂O₃ is discussed, and the relation between grain aspect ratio and mechanical properties in these materials is presented. This alloy is produced commercially by the Huntington Alloy Products Division of The International Nickel Company, Inc. as INCONELŗ alloy MA-753.     

The coarsening kinetics of γ′ particles in nickel-based alloys

The present article describes a method for calculating the coarsening rate of γ′ in Ni-based superalloys, which has been applied to both binary Ni-Al alloys and a wide range of multicomponent alloys. A standard coarsening equation is utilized, but innovative methods for calculating the critical input parameters are presented. The article details methods of estimating interfacial energies and the effective diffusion coefficients that are key parameters for the coarsening model. Self-consistent calculations are made via a computer program in which the only input required is the composition of the alloys and the temperature of coarsening. The effects of coherent strain on the coarsening process have also been analyzed and discussed.     

铁/镍基奥氏体多晶合金晶界弯曲研究进展

对于在高温环境服役的金属材料,晶界作为组织结构上的薄弱环节常常引发晶界裂纹而造成合金失效,严重影响了材料的高温力学性能表现。因而,如何改善晶界状态、提高晶界强度,是提高合金高温性能的关键。在铁/镍基奥氏体多晶合金中,采用晶界弯曲的方法强化晶界、改善合金性能一直受到国内外研究人员的广泛关注。从弯曲晶界的获得方法、形成机制及其对材料性能的影响3个方面概述了目前国内外的研究现状。较为全面地总结了特殊热处理与材料合金化等获得弯曲晶界的方法;讨论了不同合金中晶界第二相诱发晶界弯曲的驱动力和内在机理;介绍了弯曲晶界对材料力学性能、耐蚀性能及焊接性能的影响。最后,结合当前的研究现状,围绕弯曲晶界的形成条件和机制,以及弯曲晶界对性能的影响,提出了弯曲晶界未来的研究发展方向。      

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.     

Finite element analysis of cavitating facet interaction in a fully lamellar titanium aluminide alloy under creep conditions

Creep constrained grain boundary cavitation in a fully lamellar (FL) form of a titanium aluminide intermetallic alloy has been studied using finite element (FE) techniques. Two different forms of FL models were considered. Cavitation was modeled in the presence of grain boundary sliding (GBS) for the case of straight former γ grain boundaries. Models of cavitation without GBS were also performed for a FL microstructure with serrated former γ grain boundaries. The effect of cavitating facet interaction on rupture life has been studied. A comparison between the FL forms and a dualphase equiaxed microstructure having the same phase ratio (α ₂/γ) was also made to examine the relative susceptibility of these microstructures to high-temperature damage. It has been observed that the overall effect of interaction between cavitating facets increases the rupture time significantly when these facets are on adjacent grains. However, in the presence of GBS, cavitation on the facet with narrower separation effectively reduces the cavity growth rate on the facet with wider separation. This article is based on a presentation made in the symposium “Fundamentals of Gamma Titanium Aluminides,” presented at the TMS Annual Meeting, February 10–12, 1997, Orlando, Florida, under the auspices of the ASM/MSD Flow & Fracture and Phase Transformations Committees.     

高温合金晶粒细化概述

随着铸造合金尤其是铸造高温合金在工业领域内的广泛应用，多年来冶金工作者为了充分发挥合金的作用及改善合金的性能，对晶粒细化给予很大的关注，并采用了各种方法，如添加形核剂、快速冷却、工艺参数的控制、熔体在凝固过程中的机械振动和搅拌及精铸壳内表面涂层等。“ＦＧＰ”细化工艺、Ｍｉｃｒｏｃａｓｔ－Ｘ专利、Ｇｒａｉｎｅｘ专利和用ＣｏＯ＋Ａｌ２Ｏ３在精铸壳内表面涂层等已被工业采用。虽然孕育剂的添加是一种有效、简单和实用的晶粒细化方法，但直至目前，因为各种因素的限制尚未发现一种令人满意的高温合金细化添加剂。因此，靠加孕育剂细化高温合金晶粒是很困难的，目前这方面的研究仍在进行。     

Formation of Grain Boundary <Emphasis Type="Italic">α</Emphasis> in <Emphasis Type="Italic">β</Emphasis> Ti Alloys: Its Role in Deformation and Fracture Behavior of These Alloys

Beta-Ti alloys contain sufficient concentrations of β stabilizing alloy additions to permit retention of the metastable β phase after cooling to room temperature. Decomposition of the metastable β phase results in the formation of several possible phases, at least two of which are metastable. Concurrently, equilibrium α phase often forms first by heterogeneous nucleation at the α grain boundaries with an accompanying precipitate free zone observed adjacent to the grain boundary α. The grain boundary regions are softer than the precipitation hardened matrix. As a consequence, fracture follows the prior β grain boundaries, especially in high-strength conditions. This fracture mode results in low tensile ductility and/or fracture toughness. This article will describe methods of minimizing or eliminating grain boundary α formation by using metastable transition precipitates to nucleate α more rapidly. The effects on fracture behavior also will be described.     

Compressive creep behavior of spray-formed gamma titanium aluminide

The creep behavior of spray-formed γ-TiAl with a fine, equiaxed fully lamellar (FL) microstructure was studied in a temperature-stress regime of 780 °C to 850 °C and 180 to 320 MPa. An apparent stress exponent of 4.3 and an activation energy of 342 kJ/mol were observed in the high-temperature high-stress regime. Compared with the FL γ-TiAl which was obtained through conventional casting+heat treatment processes, the spray-formed γ-TiAl exhibited higher creep resistance. The higher creep resistance observed in the present study was discussed in light of the interstitial level, the chemical composition, the grain size, and the interlocking of lamellae at the grain boundary, which in turn may be a function of interlamellar spacing and the step height of the serrated grain boundaries. It was suggested that the small interlamellar spacing and possibly larger step height may contribute to the higher creep resistance observed in the present study.     

Numerical models of creep and boundary sliding mechanisms in single-phase, dual-phase, and fully lamellar titanium aluminide

Finite element simulations of the high-temperature behavior of single-phase γ, dual-phase α₂+γ, and fully lamellar (FL) α₂+γTiAl intermetallic alloy microstructures have been performed. Nonlinear viscous primary creep deformation is modeled in each phase based on published creep data. Models were also developed that incorporate grain boundary and lath boundary sliding in addition to the dislocation creep flow within each phase. Overall strain rates are compared to gain an understanding of the relative influence each of these localized deformation mechanisms has on the creep strength of the microstructures considered. Facet stress enhancement factors were also determined for the transverse grain facets in each model to examine the relative susceptibility to creep damage. The results indicate that a mechanism for unrestricted sliding of γ lath boundaries theorized by Hazzledine and co-workers leads to unrealistically high strain rates. However, the results also suggest that the greater creep strength observed experimentally for the lamellar microstructure is primarily due to inhibited former grain boundary sliding (GBS) in this microstructure compared to relatively unimpeded GBS in the equiaxed microstructures. The serrated nature of the former grain boundaries generally observed for lamellar TiAl alloys is consistent with this finding.     

Dwell-Fatigue of Ni-Based Superalloys with Serrated and Planar Grain Boundary Morphologies: The Role of the γ′ Phase on Strain Accumulation and Cavitation

The effect of grain boundary (GB) morphology on the cavitation behavior in a Ni-based superalloy, RR1000, was studied during elevated temperature dwell-fatigue at 700 °C. Following a solution heat treatment, the material was control cooled at two different rates, resulting in high angle GB morphologies that were tailored as either serrated or planar. The resulting γ′ precipitate structures were characterized near GBs and within grains. Along serrated GBs coarsened and elongated γ′ precipitates formed and consequently created adjacent regions that were denuded of γ′ precipitates. Cyclic dwell-fatigue experiments were performed at low and high stress amplitudes to vary the amount of imparted strain on the specimens. A combination of electron backscatter diffraction and digital image correlation were used to resolve strain localization relative to the GBs, in which strain accumulation was found to precede cavity formation. Additionally, the regions denuded of the γ′ precipitates were observed to localize strain and to be initial sites of cavitation. These results present a quantitative strain analysis between two variants of an RR1000 alloy, which provides the micromechanical rationale to assess the increased proclivity for serrated GBs to form cavities.

     

Directional and single-crystal solidification of Ni-base superalloys: Part II. Coincidence site lattice character of grain boundaries

The development of grain boundary misorientations with an evolving axial texture during directional solidification has been examined using the electron backscattered diffraction (EBSD) technique on the Ni-base superalloys, CMSX4 and CM186LC. A preferred grain boundary misorientation distribution (GBMD) for a sharp 〈001〉 axial texture in CM186LC was associated with a clustering of misorientation axes (MAx) in the proximity of 〈001〉. This is accompanied by an enhanced distribution of coincidence site lattice (CSL) boundaries. The increased distribution of low angle boundaries, Σ1 and Σ5, can be attributed to the existence of a preferred MAx and accommodation by secondary intrinsic grain boundary dislocations. The more diffuse 〈001〉 axial texture in CMSX4 is associated with a significant proportion of MAx deviating from 〈001〉 and a dramatic reduction in the proportion of CSL boundaries.     

The Effect of Friction Stir Processing on the Mechanical Properties of Investment Cast and Hot Isostatically Pressed Ti-6Al-4V

Friction-stir (FS) processing was used to modify the coarse, fully lamellar microstructure of investment cast and hot isostatically pressed (HIP’ed) Ti-6Al-4V. The effect of FS processing on mechanical properties was investigated using microtensile and four-point bend fatigue testing. The tensile results showed a typical microstructure dependence where yield strength and ultimate tensile strength both increased with decreasing slip length. Depending on the processing parameters, fatigue strength at 10⁷ cycles was increased by 20 pct or 60 pct over that of the investment cast and HIP’ed base material. These improvements have been verified with a statistically significant number of tests. The results have been discussed in terms of the resistance of each microstructure fatigue crack initiation and small crack propagation. For comparison, a limited number of fatigue tests was performed on α + β forged Ti-6Al-4V with varying primary α volume fraction and also on investment cast material heat treated to produce a bi-lamellar condition.     

The effect of γ′ content on the densities of Ni-based superalloys

The γ′ phase increases the mechanical strength of Ni-based superalloys. Equations have been derived to calculate the atomic percent of γ′ phase from the Al content of the alloy. It is shown that increased γ′ phase content results in an increase in density (of the solid) and a decrease in the thermal expansion coefficient. Equations based on the Al content of the alloy have been derived to calculate the magnitude of these effects. The coarsening of the γ′ phase from 800 °C to 1000 °C was found to be accompanied by an increase in the temperature dependence of the thermal expansion coefficient. Densities for the entire temperature range of the solid alloys calculated with the equations are within 2 pct of measured values. The strong bonding between the Ni and Al was maintained in the liquid and resulted in increased densities. Equations were derived to quantify the effect on density (of the liquid) and the calculated density values for Ni-based superalloys were within 2 pct of the measured values. These uncertainties are commensurate with the experimental uncertainty in the measurements.     

On the Role of Grain Boundary Serration in Simulated Weld Heat-Affected Zone Liquation of a Wrought Nickel-Based Superalloy

The effects of grain boundary serration on boron segregation and liquation cracking behavior in a simulated weld heat-affected zone (HAZ) of a wrought nickel-based superalloy 263 have been investigated. The serrated grain boundaries formed by the developed heat treatment were highly resistant to boron segregation; the serrated sample contained 41.6 pct grain boundaries resistant to boron enrichment as compared with 14.6 pct in the unserrated sample. During weld thermal cycle simulation, liquated grain boundaries enriched with boron were observed at the peak temperature higher than 1333 K (1060 °C) in both unserrated and serrated samples; however, serrated grain boundaries exhibited a higher resistance to liquation. The primary cause of liquation in this alloy was associated with the segregation of the melting point depressing element boron at grain boundaries. The hot ductility testing result indicated that the serrated grain boundaries showed a lower susceptibility to liquation cracking; the grain boundary serration led to an approximate 15 K decrease in the brittle temperature range. These results reflect closely a significant decrease in interfacial energy as well as a grain boundary configuration change by the serration.     

Mechanism of primary MC carbide decomposition in Ni-base superalloys

Three industrial gas turbine blades made of conventionally cast (CC) IN-738 and GTD-111 and directionally solidified GTD-111 Ni-base superalloys were examined after long-term exposures in service environments. All three blades exhibit similar, service-induced microstructural changes (MCs) including γ′ coarsening and coalescence, excessive secondary M₂₃C₆ precipitation, and primary MC degeneration, regardless of the chemical composition and the grain size. Special attention was paid to the primary MC decomposition. It is shown that the primary MC decomposition occurs by carbon diffusion out of the carbide into the γ + γ′ matrix, resulting in the formation of Cr-rich M₂₃C₆ carbides near the initial carbide/matrix interface. A transition zone is shown to develop between the original MC core and its perimeter, demonstrating the gradual outward diffusion of carbon and a slight inward increase in nickel concentration. The hexagonal Ni₃(TiTa) η-phase was also found in the MC transition zone and on the MC-γ/γ′ interface. The primary MC decomposition can be expressed by the reaction MC + γ/γ′ → M₂₃C₆ + η. Finally, it is shown that the grain-boundary (GB) MC decomposes more rapidly than that in the grain interiors. This is consistent with the more rapid GB diffusion that leads to the acceleration of the MC diffusional decomposition processes.     

Grain Boundary Curvature in a Model Ni-Based Superalloy

The local grain boundary (GB) curvature in a model Ni-based superalloy was measured experimentally using Dehoff’s tangent count method. The results show that, in materials containing significant amounts of second-phase particles, the curvature parameter, κ, which relates the mean local curvature to the grain size, can adopt far lower values than have been reported previously. It is also shown that the value of κ is not a constant, as is usually assumed, but instead varies both with the volume fraction of second-phase particles and with the holding time during high-temperature annealing. The lowest values for κ were obtained for high particle volume fractions and long annealing times. Because the local boundary curvature constitutes the driving force for grain growth, these observations could help to explain grain growth phenomena in heavily pinned systems.

---