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The effect of adding 2 at.% W to a model Ni-Al-Cr superalloy on the morphological evolution, spatial correlations and temporal evolution of g'(L12)-precipitates at 1073 K is studied with scanning electron microscopy and atomic force microscopy. Adding W yields a larger microhardness, earlier onset of spheroidal-to-cuboidal precipitate morphological transition, larger volume fraction (from ~20 to 30%), reduction in coarsening kinetics by one third and a larger number density (Nv) of smaller mean radii () precipitates. The kinetics of and interfacial area per unit volume obey t1/3 and t-1/3 relationships, respectively, which is consistent with coarsening driven by interfacial energy reduction. The Nv power law dependencies deviate, however, from model predictions indicating that a stationary-state is not achieved. Quantitative analyses with precipitate size distributions, pair correlation functions, and edge-to-edge interprecipitate distance distributions gives insight into 2D microstructural evolution, including the elastically driven transition from a uniform g'-distribution to one-dimensional <001>-strings to eventually clustered packs of g'-precipitates in the less densely packed Ni-Al-Cr alloy., Comment: in-press, Acta Materialia: 44 pages, 15 figures (double spaced Word document)

The kinetic pathways resulting from the formation of coherent L12-ordered y'-precipitates in the g-matrix (f.c.c.) of Ni-7.5 Al-8.5 Cr at.% and Ni-5.2 Al-14.2 Cr at.% alloys, aged at 873 K, are investigated by atom-probe tomography (APT) over a range of aging times from 1/6 to 1024 hours; these alloys have approximately the same volume fraction of the y'-precipitate phase. Quantification of the phase decomposition within the framework of classical nucleation theory reveals that the y-matrix solid-solution solute supersaturations of both alloys provide the chemical driving force, which acts as the primary determinant of the nucleation behavior. In the coarsening regime, the temporal evolution of the y'-precipitate average radii and the y-matrix supersaturations follow the predictions of classical coarsening models, while the temporal evolution of the y'-precipitate number densities of both alloys do not. APT results are compared to equilibrium calculations of the pertinent solvus lines determined by employing both Thermo-Calc and Grand-Canonical Monte Carlo simulation., Comment: Submitted to Acta Materialia, June, 2007

An algorithm is presented to fit precipitates in atom probe tomographic data sets as equivalent ellipsoids. Unlike previous techniques, which measure only the radius of gyration, these ellipsoids retain the moments of inertia and principle axes of the original precipitate, preserving crystallographic orientational information. The algorithm is applied to study interconnected gamma prime precipitates (L1_2) in the Gamma-matrix (FCC) of a Ni-Al-Cr alloy. The precipitates are found to coagulate along <110>-type directions., Comment: Accepted for publication in Scripta Materialia, added information about local magnification effects

The chemical pathways leading to gamma-prime(L1_2)-nucleation from nondilute Ni-5.2 Al-14.2 Cr at.%, gamma(f.c.c.), at 873 K are followed with radial distribution functions and isoconcentration surface analyses of direct-space atom-probe tomographic images. Although Cr atoms initially are randomly distributed, a distribution of congruent Ni3Al short-range order domains (SRO), =0.6 nm, results from Al diffusion during quenching. Domain site occupancy develops as their number density increases leading to Al-rich phase separation by gamma-prime-nucleation, =0.75 nm, after SRO occurs., Comment: 5 pages, 4 figures

Powder-bed additive manufacturing processes use fine powders to build parts layer-by-layer. Alloy 718 powder feedstocks for selective laser melting (SLM) additive manufacturing are produced commercially by both gas and rotary atomization and are available typically in the 10-45 or 15-45 microns size ranges. A comprehensive investigation was conducted to understand the impact of powder variability on the microstructure and mechanical behavior of SLM 718 heat treated to Aerospace Material Specification (AMS) 5664. This study included sixteen virgin powders and three once-recycled powders within the 10-45 and 15-45 microns size ranges that were obtained from seven direct source suppliers and one reseller. Although alike as highly regular spheroids, these powders showed distinct differences in composition (especially Al, C and N contents), particle size distributions, and powder features such as degree of agglomeration, fusion and surface roughness. Compositional differences expectedly had the strongest impact on microstructure. High N and C contents formed TiN-nitrides and/or (Nb,Ti,Mo)-C carbides on the grain boundaries, prevented recrystallization during heat treatment, and resulted in retained (001)-scalloped shaped grains that ranged from 19 to 41 microns in average size. In the absence of this particle pinning, the average grain size of the heat treated SLM 718 ranged from 51 microns to 90 microns. Room temperature tensile and high cycle fatigue (HCF) testing compared as-fabricated (AF) and low stress ground (LSG) surface conditions. Tensile testing revealed consistent behavior between the two surface conditions and amongst the powder lots. The finer grained SLM 718 builds displayed the lowest tensile properties. A SLM 718 build fabricated from a powder with eight times lower C content showed statistically better tensile properties presumably due to enhanced coarsening of (delta)-Ni3Nb precipitates. The specimens from once-recycled powders had slightly higher tensile strengths and slightly higher ductility compared to their virgin equivalents; once-recycling also did not substantially degrade the mean HCF life. The LSG fatigue lives agreed with conventionally manufactured 718 data, while AF lives exhibited a knock-down due to surface roughness. The fatigue lives of AF specimens were statistically equivalent across powder lots except for one and failures typically initiated at stress concentrators associated with SLM surface asperities. Fatigue testing of low stress ground specimens result in both transgranular and within facet crack initiations. More than half of the cracks initiated from these facets for the machined condition; however, these facets appeared to be within grains that were larger-than-average in size. A nitrogen-atomized powder with fine prior particles of TiN-nitrides and M(Ti,Nb,Mo)C carbides from atomization on powder surfaces resulted in the best fatigue performance with segregation of these particles to the SLM 718 grain boundaries leading to higher resistance to early-stage crack propagation. Typically the fine-grained builds with minor phases along the grain boundaries did not perform well in fatigue, whereas a larger-grain build with lower carbon content and coarser delta-Ni3Nb precipitates showed the next best HCF response. Further details of the build microstructure and its impact on tensile and fatigue behavior was considered.

Examine set-to-set variability with 4 build sets with the same layout Establish the effect of solutioning heat treatments (HT) on as-fabricated grain structure and microstructure – (gamma)’-solvus= 1156 ºC (1) As-fabricated (2) 2 hour subsolvus HT(-15 ºC) + conventional 2-step aging (3, 4, 5) 0.5 hour, 2 hours, 4 hours supersolvus HT (+18 ºC) + 2 step aging Gain insight into location-specific microstructure to correlate later to mechanical properties (tensile, creep, LCF behavior)

Superalloy 718 is an excellent candidate for selective laser melting (SLM) fabrication due to a combination of excellent mechanical properties and workability. Predicting and validating the microstructure of SLM-fabricated Superalloy 718 after potential post heat-treatment paths is an important step towards producing components comparable to those made using conventional methods. At present, obtaining accurate volume fraction and size measurements of gamma-double-prime, gamma-prime and delta precipitates has been challenging due to their size, low volume fractions, and similar chemistries. A technique combining high resolution distortion corrected SEM imaging and with x-ray energy dispersive spectroscopy has been developed to accurately and independently measure the size and volume fractions of the three precipitates. These results were further validated using x-ray diffraction and phase extraction methods and compared to the precipitation kinetics predicted by PANDAT and JMatPro. Discrepancies are discussed in context of materials properties, model assumptions, sampling, and experimental errors.

Powder-bed fabrication of aerospace alloys may revolutionize production by eliminating the need for extensive machining and expensive tooling. Heated-bed electron-beam melting (EBM) offers advantages over non-heated laser additive manufacturing (AM) methods, including lower residual stress, reduced risk of contamination, slower cooling rates, and faster build times. NASA Glenn Research Center has joint project work with Oak Ridge National Lab and the Air Force Research Laboratory to explore the feasibility of fabricating advanced Ni-based gamma-prime superalloys with EBM AM.

Powder metallurgy disk superalloys have been designed for higher engine operating temperatures through improvement of their strength and creep resistance. Yet, increasing disk application temperatures to 704 degrees Centigrade and higher could enhance oxidation and activate hot corrosion in harmful environments. Protective coatings could be necessary to mitigate such attack. Cylindrical coated specimens of disk superalloys LSHR and ME3 were subjected to thermal cycling to produce cyclic oxidation in air at a maximum temperature of 760 degrees Centigrade. The effects of substrate roughness and coating thickness on coating integrity after cyclic oxidation were considered. Selected coated samples that had cyclic oxidation were then subjected to accelerated hot corrosion tests. This cyclic oxidation did not impair the coating's resistance to subsequent hot corrosion pitting attack.

The mechanical properties of several cast blade superalloys and one powder metallurgy disk superalloy were assessed for potential use in a dual alloy hybrid disk concept of joined dissimilar bore and web materials. Grain size was varied for each superalloy class. Tensile, creep, fatigue, and notch fatigue tests were performed at 704 to 815 degC. Typical microstructures and failure modes were determined. Preferred materials were then selected for future study as the bore and rim alloys in this hybrid disk concept. Powder metallurgy superalloy LSHR at 15 micron grain size and single crystal superalloy LDS-1101+Hf were selected for further study, and future work is recommended to develop the hybrid disk concept.

Environmental attack has the potential to limit turbine disk durability, particularly in next generation engines which will run hotter; there is a need to understand better oxidation at potential service conditions and develop models that link microstructure to fatigue response. More efficient gas turbine engine designs will require higher operating temperatures. Turbine disks are regarded as critical flight safety components; a failure is a serious hazard. Low cycle fatigue is an important design criteria for turbine disks. Powder metallurgy alloys, like ME3, have led to major improvements in temperature performance through refractory additions (e.g. Mo,W) at the expense of environmental resistance (Al, Cr). Service conditions for aerospace disks can produce major cycle periods extending from minutes to hours and days with total service times exceeding 1,000 hours in aerospace applications. Some of the effects of service can be captured by extended exposures at elevated temperature prior to LCF testing. Some details of the work presented here have been published.

Mechanical property requirements vary with location in nickel-based superalloy disks. In order to maximize the associated mechanical properties, heat treatment methods have been developed for producing tailored grain microstructures. In this study, fatigue failure modes of a grain size transition zone in a dual microstructure disk were evaluated. A specialized heat treatment method was applied to produce varying grain microstructure in the bore to rim portions of a powder metallurgy processed nickel-based superalloy disk. The transition in grain size was concentrated in a zone of the disk web, between the bore and rim. Specimens were extracted parallel and transversely across this transition zone, and multiple fatigue tests were performed at 427 C and 704 C. Grain size distributions were characterized in the specimens, and related to operative failure initiation modes. Mean fatigue life decreased with increasing maximum grain size, going out through the transition zone. The scatter in limited tests of replicates was comparable for failures of uniform gage specimens in all transition zone locations examined.

Oxidation and the effects of high temperature exposures on notched fatigue life were considered for a powder metallurgy processed supersolvus heat-treated ME3 disk superalloy. The isothermal static oxidation response at 704 C, 760 C, and 815 C was consistent with other chromia forming nickel-based superalloys: a TiO2-Cr2O3 external oxide formed with a branched Al2O3 internal subscale that extended into a recrystallized - dissolution layer. These surface changes can potentially impact disk durability, making layer growth rates important. Growth of the external scales and dissolution layers followed a cubic rate law, while Al2O3 subscales followed a parabolic rate law. Cr- rich M23C6 carbides at the grain boundaries dissolved to help sustain Cr2O3 growth to depths about 12 times thicker than the scale. The effect of prior exposures was examined through notched low cycle fatigue tests performed to failure in air at 704 C. Prior exposures led to pronounced debits of up to 99 % in fatigue life, where fatigue life decreased inversely with exposure time. Exposures that produced roughly equivalent 1 m thick external scales at the various isotherms showed statistically equivalent fatigue lives, establishing that surface damage drives fatigue debit, not exposure temperature. Fractographic evaluation indicated the failure mode for the pre-exposed specimens involved surface crack initiations that shifted with exposure from predominately single intergranular initiations with transgranular propagation to multi-initiations from the cracked external oxide with intergranular propagation. Weakened grain boundaries at the surface resulting from the M23C6 carbide dissolution are partially responsible for the intergranular cracking. Removing the scale and subscale while leaving a layer where M23C6 carbides were dissolved did not lead to a significant fatigue life improvement, however, also removing the M23C6 carbide dissolution layer led to nearly full recovery of life, with a transgranular initiation typical to that observed in unexposed specimens.

For a Ni-5.2 Al-14.2 Cr at.% alloy with moderate solute supersaturations, the compositional pathways, as measured with atom-probe tomography, during early to later stage y'(LI2)-precipitation (R = 0.45-10 nm), aged at 873 K, are discussed in light of a multi-component coarsening model. Employing nondilute thermodynamics, detailed model analyses during quasistationary coarsening of the experimental data establish that the y/y' interfacial free-energy is 22- 23+/-7 mJ/sq m. Additionally, solute diffusivities are significantly slower than model estimates. Strong quantitative evidence indicates that an observed y'-supersaturation of Al results from the Gibbs-Thomson effect, providing the first experimental verification of this phenomenon. The Gibbs-Thomson relationship, for a ternary system, as well as differences in measured phase equilibria with CALPHAD assessments, are considered in great detail.

The chemical pathways leading to gamma'(L1(sub 2)) nucleation from nondilute Ni-5.2 Al-14.2 Cr at. %, gama(fcc), at 873 K are followed with radial distribution functions and isoconcentration surface analyses of direct-space atom-probe tomographic images. Although Cr atoms initially are randomly distributed, a distribution of congruent Ni3Al short-range-order domains (SRO), [R] approx. equals 0.6 nm, results from Al diffusion during quenching. Domain site occupancy develops as their number density increases leading to Al-rich phase separation by gamma'-nucleation, [R]=0.75 nm, after SRO occurs.

Early-stage phase separation in a Ni-5.2 Al-14.2 Cr at.% superalloy, isothermally decomposing at 873 K, is investigated with atom-probe tomography. Sub-nanometer scale compositional profiles across the gamma/gamma'(L12) interfaces demonstrate that both the gamma-matrix and the gamma'-precipitate compositions evolve with time. Observed chemical gradients of Al depletion and Cr enrichment adjacent to the gamma'-precipitates are transient, consistent with well-established model predictions for diffusion-limited growth, and mark the first detailed observation of this phenomenon. Furthermore, it is shown that Cr atoms are kinetically trapped in the growing precipitates.

The influence of W on the temporal evolution of gamma' precipitation toward equilibrium in a model Ni-Al-Cr alloy is investigated by three-dimensional atom-probe (3DAP) microscopy and transmission electron microscopy (TEM). We report on the alloys Ni-10 Al-8.5 Cr (at.%) and Ni-10 Al-8.5 Cr-2 W (at.%), which were aged isothermally in the gamma + gamma' two-phase field at 1073 K, for times ranging from 0.25 to 264 h. Spheroidal-shaped gamma' precipitates, 5-15 nm diameter, form during quenching from above the solvus temperature in both alloys at a high number density (approx. 10(exp 23/cu m). As gamma' precipitates grow with aging at 1073 K, a transition from spheriodal- to cuboidal-shaped precipitates is observed in both alloys. The elemental partitioning and spatially resolved concentration profiles across the gamma' precipitates are obtained as a function of aging time from three-dimensional atom-by-atom reconstructions. Proximity histogram concentration profiles of the quaternary alloy demonstrate that W concentration gradients exist in gamma' precipitates in the as-quenched and 0.25-h aging states, which disappear after 1 h of aging. The diffusion coefficient of W in gamma' is estimated to be 6.2 x 10(exp -20) sq m/s at 1073 K. The W addition decreases the coarsening rate constant, and leads to stronger partitioning of Al to gamma' and Cr to gamma.

The early to the later stages of precipitation of ordered gamma'-precipitates (L1(sub 2)) in Ni-5.2 Al-14.2 Cr (at.%) are studied at 873 K. Precipitates with radii as small as 0.45 nm are characterized fully by three-dimensional atom-probe (3DAP) microscopy. Contrary to what is often assumed by theory or in models, the average precipitate composition is shown to evolve with time, such that solute concentrations decrease toward an equilibrium value given by the solvus lines. Power-law time dependencies of the number density, mean radius, and supersaturations of Al and Cr are discussed in light of theoretical predictions for Ostwald ripening.

The temporal evolution of the nanostructure of a model Ni-base superalloy (Ni-5.2 at.% Al-14.2 at.% Cr) is studied experimentally employing three-dimensional atom-probe (3DAP) microscopy in conjunction with kinetic Monte Carlo (KMC) simulations at 600 C. It is demonstrated that not only can the mean compositions of individual gamma' (Ni3Al with the Li2 structure) precipitates be measured but the Ni, Al, and Cr concentration profiles within the precipitates can also be determined for precipitates with a mean radius () as small as 0.85 nm. The three asymptotic tinie dependencies of the Lifshitz-Slyzov-Wagner (LSW) theory of coarsening (Ostwald ripening) are measured and found to deviate from its theoretical predictions: possible explanations for these discrepancies are discussed. At 0.25 hr. there is 3DAP microscope evidence for the presence of precipitates of another nickel-rich phase. ="Ni3Cr" (Ni3Cr(1-x)Al(x)), which exhibits short-range order (SRO) and that is metastable with respect to Ni3Al. This metastable phase is also found by KMC simulations and has the composition Ni3Cr(1-x)Al(x), which is Ni-2.91 at.% Al-21.98 at.% Cr at 16 hours. Our results demonstrate that the decomposition of gamma the primary gamma (FCC) phase results in the concurrent formation of an ordered phase and a disordered phase by 0.25 hours.