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All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Creep Behavior of a High-$\gamma^{\prime}$ Ni-Based Superalloy Fabricated via Electron Beam Melting

Additive manufacturing enables the fabrication of complex engineering components previously inaccessible through traditional processes. Nickel-base superalloys with large γ' volume fraction are typically considered non-weldable and therefore exhibit a propensity for cracking during the fusion process. These crack-prone materials, however, are of great importance in gas turbine engines due to their excellent high temperature creep resistance. In this study we investigate the creep behavior of IN738LC produced by the electron beam melting process. Here, we find that with appropriate post-build heat treatment the creep response of material oriented in the build direction exhibits deformation and rupture behavior comparable to that of conventionally cast IN738 & IN738LC. In the transverse direction properties fall below the expected cast behavior, however, we argue this is likely due to differences in grain scale and crystallographic texture. It may be possible to coarsen the grain morphology with appropriate process-parameter optimization in order to reduce the severity of intergranular fracture in the transverse direction. These results illustrate that high temperature properties exhibited by additively manufactured IN738LC are suitable for the hot section of gas turbine engines.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Evolution of micro-pores in Ni–Cr alloys via molten salt dealloying

Porous materials with high specific surface area, high porosity, and high electrical conductivity are promising materials for functional applications, including catalysis, sensing, and energy storage. Molten salt dealloying was recently demonstrated in microwires as an alternative method to fabricate porous structures. The method takes advantage of the selective dissolution process introduced by impurities often observed in molten salt corrosion. This work further investigates molten salt dealloying in bulk Ni–20Cr alloy in both KCl–MgCl 2 and KCl–NaCl salts at 700 °C, using scanning electron microscopy, energy dispersive spectroscopy, and X-ray diffraction (XRD), as well as synchrotron X-ray nano-tomography. Micro-sized pores with irregular shapes and sizes ranging from sub-micron to several microns and ligaments formed during the process, while the molten salt dealloying was found to progress several microns into the bulk materials within 1–16 h, a relatively short reaction time, enhancing the practicality of using the method for synthesis. The ligament size increased from ~ 0.7 μm to ~ 1.3 μm in KCl–MgCl 2 from 1 to 16 h due to coarsening, while remaining ~ 0.4 μm in KCl–NaCl during 16 h of exposure. The XRD analysis shows that the corrosion occurred primarily near the surface of the bulk sample, and Cr 2 O 3 was identified as a corrosion product when the reaction was conducted in an air environment (controlled amount sealed in capillaries); thus surface oxides are likely to slow the morphological coarsening rate by hindering the surface diffusion in the dealloyed structure. 3D-connected pores and grain boundary corrosion were visualized by synchrotron X-ray nano-tomography. This study provides insights into the morphological and chemical evolution of molten salt dealloying in bulk materials, with a connection to molten salt corrosion concerns in the design of next-generation nuclear and solar energy power plants.

36 MATERIALS SCIENCE↗
NASA NTRS1987

Growth process of gamma'-particles in a liquid-quenched Ni-15 at percent Al alloy

The growth of gamma-prime particles in a supersaturated Ni-15 at% Al alloy prepared by the liquid-quench method was studied using a magnetic mass balance, transmission electron microscopy, and field ion microscopy. Three stages in the precipitation and growth of these particles are demonstrated. In the first phase, the gamma-prime phase was produced by nucleation of spinodal decomposition of the alloy. In the second stage, spherical gamma-prime particles were arranged at random in the matrix with the size independent of aging time. Then, the Al concentration in the matrix decreased with the -1/3 power of the aging time. These results suggest that the degree of ordering increases with aging time. In the third stage, the particles were coarsened with aging time. They were arranged in the matrix (100) zone and were cubic, with the cube face lying on (100). The interfacial free energy was 28.4 mJ/sq m at 873 K and 22.4 mJ/sq m at 973 K.

Tachikake, A.↗
DOE OSTI2024

Dissolution zone model of the oxide structure in additively manufactured dispersion-strengthened alloys

The structural evolution of oxides in dispersion-strengthened superalloys during laser-powder bed fusion is considered in detail. Alloy chemistry and process parameter effects on oxide structure are assessed through a parameter study on the model alloy Ni-20Cr, doped with varying concentrations of Y 2 O 3 and Al. Small angle neutron scattering measurements of the dispersoid size distribution show the dispersoid size increases with higher laser power, slower scan speed, and increasing Y 2 O 3 and Al content. Complementary electron microscopy measurements reveal reactions between Y 2 O 3 and Al, even in nanoscale dispersoids, and the presence of micron-scale oxide slag inclusions in select specimens. A scaling analysis of mass and momentum transport within the melt pool, presented here, establishes that diffusional structural evolution mechanisms dominate for nanoscale dispersoids, while fluid forces and advection become significant for larger slag inclusions. These findings are developed into a theory of dispersoid structural evolution, integrating quantitative models of diffusional processes – dispersoid dissolution, nucleation, growth, coarsening – with a reduced order model of time-temperature trajectories of fluid parcels within the melt pool. Calculations of the dispersoid size in single-pass melting reveal a zone in the center of the melt track in which the oxide feedstock fully dissolves. Within this zone the final Y 2 O 3 size is independent of feedstock size and determined by nucleation and growth kinetics. If the dissolution zones of adjacent melt tracks overlap sufficiently with each other to dissolve large oxides, formed during printing or present in the powder feedstock, then the dispersoid structure throughout the build volume is homogeneous and matches that from a single pass within the dissolution zone. Gaps between adjacent dissolution zones result in oxide accumulation into larger slag inclusions. Predictions of final dispersoid size and slag formation using this dissolution zone model match the present experimental data and explain process-structure linkages speculated in the open literature.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Variations in γ′ formers and refractory elements for enhanced creep resistance and phase stability of an advanced Ni-based superalloy

The strong demands on increasing fuel efficiency have continuously driven the optimization of superalloys for high-performance applications. In this study, modifications to the chemistry and heat treatment of HAYNES® 282® alloy (H282) were performed by varying γ′ formers and refractory elements. It was found that increasing Ti and substituting W for some of the Mo in the newly designed alloy (Q) resulted in a significant improvement of creep resistance, up to 130% increase in creep life, compared to standard H282. It was found that Orowan loops and dislocation climb were the dominant creep deformation mechanisms in alloy Q, while extensive dislocation tangling as an additional configuration was observed in the baseline alloy. Moreover, phase stability investigations for up to 5000 h at 800 °C and 900 °C revealed a reduced formation of detrimental σ and μ phases in alloy Q when compared to H282. Atom-probe tomography (APT) revealed that the formation and growth of those phases were responsible for a decrease in Mo content in the matrix, thereby leading to a decrease in solid-solution strengthening in H282 over time. Furthermore, the coarsening of γ′ precipitates was retarded by the substitution of W for Mo, particularly under creep stress. The theoretical and experimental understanding of precipitation strengthening unraveled that higher optimal strengthening occurs at larger particle size for alloy Q, compared to the commercial formulation, further explaining the origin of enhanced creep resistance in the modified alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Rafting-Enabled Recovery Avoids Recrystallization in 3D-Printing-Repaired Single-Crystal Superalloys

The repair of damaged Ni-based superalloy single-crystal turbine blades has been a long-standing challenge. Additive manufacturing by an electron beam is promising to this end, but there is a formidable obstacle: either the residual stress and γ/γ' microstructure in the single-crystalline fusion zone after e-beam melting are unacceptable (e.g., prone to cracking), or, after solutionizing heat treatment, recrystallization occurs, bringing forth new grains that degrade the high-temperature creep properties. Here, a post-3D printing recovery protocol is designed that eliminates the driving force for recrystallization, namely, the stored energy associated with the high retained dislocation density, prior to standard solution treatment and aging. The post-electron-beam-melting, pre-solutionizing recovery via sub-solvus annealing is rendered possible by the rafting (i.e., directional coarsening) of γ' particles that facilitates dislocation rearrangement and annihilation. The rafted microstructure is removed in subsequent solution treatment, leaving behind a damage-free and residual-stress-free single crystal with uniform γ' precipitates indistinguishable from the rest of the turbine blade. Finally, this discovery offers a practical means to keep 3D-printed single crystals from cracking due to unrelieved residual stress, or stress-relieved but recrystallizing into a polycrystalline microstructure, paving the way for additive manufacturing to repair, restore, and reshape any superalloy single-crystal product.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Friction surface layer deposition of triple-phase Al 10 Cr 12 Fe 35 Mn 23 Ni 20 high entropy alloy: Process optimization and microstructural evolution

A high-strength Co-free triple-phase Al 10 Cr 12 Fe 35 Mn 23 Ni 20 high-entropy alloy (HEA) was successfully fabricated using Friction Surface Layer Deposition (FSLD), a bulk manufacturing method. Multiple single-layer deposits were produced by varying forging force (F) and traverse speeds (T r ) to optimize the process parameters. The optimized conditions (F = 40 kN & T r = 200 mm/min) were then applied to manufacture a scaled-up multi-layer specimen. The initial microstructure of the HEA consisted of coarse grains of the soft FCC-phase, long columnar dendrites of the hard BCC-phase, and small precipitates of the harder B2-phase within the BCC-dendrites. During FSLD, the FCC-matrix underwent continuous dynamic recrystallization due to high-temperature severe plastic deformation, forming finer equiaxed grains. Simultaneously, the BCC-dendrites fractured into smaller fragments, some of which experienced partial growth and coarsening under applied stress, resulting in an hourglass morphology. In contrast, the small B2-precipitates within the BCC-fragments dissolved during the elevated temperatures of FSLD and reprecipitated as substantially finer precipitates during continuous cooling post-FSLD. Additionally, the orientation relationships between the FCC and BCC/B2 phases were completely destroyed by the severe thermoplastic deformation inherent to FSLD. The microstructural refinements led to a substantial improvement in hardness from 177 HV to 283 HV, driven by Hall-Petch strengthening. The increased number of interfaces, including coherent BCC-B2 interfaces, potentially enhances the sink strength and radiation tolerance of the HEA, making it a promising candidate for nuclear applications. In conclusion, this study also highlights FSLD as a versatile technique for achieving tunable properties in HEAs, with detailed schematics illustrating the complex mechanisms of phase transformations during processing.

Additive Manufacturing↗
DOE OSTI2023

The influence of chemical short-range order on the nanoindentation properties of high-entropy alloys prepared via laser powder bed fusion

Chemical short-range order (CSRO) plays an instrumental role in determining the mechanical properties of high-entropy alloys (HEAs). Current methods for controlling CSRO mainly focus on cast HEAs, which can not solve the problem of grain coarsening caused by homogenization treatments. Laser Powder Bed Fusion (LPBF), which has extremely high cooling rates, can suppress compositional segregation, refine grain structures, and achieve low CSRO. This offers a promising avenue for quantitatively controlling CSRO without the need for homogenization treatments. In this study, we investigate the CSRO of HEAs fabricated via LPBF and elucidate their influence on nanoindentation behavior. The results show that, at the low cooling rate, the average size of CSRO is 0.66 nm and they occupy 2.8% of the cross-sectional area, while at high cooling rate, the corresponding values are 0.92 nm and 9.9%, respectively, both of which are significantly smaller than those of cast HEAs. Furthermore, by analyzing samples with different CSROs, we observe that the hardness increases and then decreases with the increase of CSRO, primarily due to the preferential formation of dislocations in regions enriched with Cr-Mn-Ni. With the improvement of CSRO, both the size and quantity of Cr-Mn-Ni rich region gradually increased; subsequently, as multiple Cr-Mn-Ni rich regions tend to merge into one during the CSRO improvement, the size of the Cr-Mn-Ni rich region continued to increase while the quantity gradually decreased; when the size of the Cr-Mn-Ni rich region is moderate and widely dispersed, the dislocation density is higher with much more uniform distributions, which favorably improves nanoindentation hardness.

36 MATERIALS SCIENCE↗
NASA NTRS2004

The Influence of Tungsten on the Chemical Composition of a Temporally Evolving Nanostructure of a Model Ni-Al-Cr Superalloy

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.

Sudbrack, Chantal K.↗
NASA NTRS2005

Ar-Ar and I-Xe Ages and the Thermal History of IAB Meteorites

Studies of several samples of the large Caddo County IAB iron meteorite reveal andesitic material, enriched in Si, Na, Al and Ca, which is essentially unique among meteorites. This material is believed to have formed from a chondritic source by partial melting and to have further segregated by grain coarsening. Such an origin implies extended metamorphism of the IAB parent body. New Ar-39- Ar-40 ages for silicate from three different Caddo samples are consistent with a common age of 4.50-4.51 Gyr ago. Less well defined Ar-Ar degassing ages for inclusions from two other IABs, EET8333 and Udei Station, are approx.4.32 Gyr, whereas the age for Campo del Cielo varies considerably over approx.3.23-4.56 Gyr. New I-129-Xe-129 ages for Caddo County and EET8333 are 4557.9+/-0.1 Myr and 4557-4560 Myr, respectively, relative to an age of 4562.3 Myr for Shallowater. Considering all reported Ar-Ar degassing ages for IABs and related winonaites, the range is approx.4.32-4.53 Gyr, but several IABs give similar Ar ages of 4.50-4.52 Gyr. We interpret these older Ar ages to represent cooling after the time of last significant metamorphism on the parent body, and the younger ages to represent later 40Ar diffusion loss. The older Ar-Ar ages for IABs are similar to Sm-Nd and Rb-Sr isochron ages reported in the literature for Caddo County. Considering the possibility that IAB parent body formation was followed by impact disruption, reassembly, and metamorphism (e.g., Benedix et al. 2000), the Ar-Ar ages and IAB cooling rates deduced from Ni concentration profiles in IAB metal (Herpfer et al., 1994) are consistent if the time of the post-assembly metamorphism was as late as approx.4.53 Gyr ago. However, I-Xe ages reported for some IABs define much older ages of approx.4558-4566 Myr, which cannot easily be reconciled with the much younger Ar-Ar and Sm-Nd ages. An explanation for the difference in radiometric ages of IABs may reside in combinations of the following: a) I-Xe ages have very high closure temperatures and were not reset during metamorphism approx.4.53 Gyr ago; b) a bias exists in the 40K decay constants which makes these Ar-Ar ages approx.30 Myr too young; c) the reported Sm-Nd and Rb-Sr ages for Caddo are in error by amounts equal to or exceeding their reported 2-sigma uncertainties; and d) about 30 Myr after the initial heating that produced differentiation of Caddo silicate and mixing of silicate and metal, a mild metamorphism of the IAB parent body reset the Ar-Ar ages.

Bogard, Donald D.↗
DOE OSTI2022

Evolution of carbide precipitates in Haynes® 282 superalloy processed by wire arc additive manufacturing

Precipitation hardening regulated with heat treatments is a critical technique for tuning the mechanical properties of Ni-based superalloys fabricated with additive manufacturing, where mechanical deformation is no longer viable for microstructural refinement. As one of the key precipitates, carbides prevail in the additively manufactured alloys, whose precipitation kinetics remain largely vague. This work studies the influence of heat treatments on the evolution of MC- and M 23 C 6 -type carbides within a Haynes® 282 superalloy prepared by wire arc additive manufacturing (WAAM). SEM-EDS analysis was performed to identify the evolution pathways of the carbides, and TEM and XRD characterizations were carried out to track the crystallographic features. The MC-type carbides are originally present in the as-printed alloy, which distribute uniformly across the whole material and remain largely unchanged in size during the heat treatments. By contrast, the incipiently non-existent M 23 C 6 -type carbides precipitate during an aging treatment at 1010 °C, which majorly extend along the grain boundaries as kinetically feasible sites. Further experimental and computational analysis confirms the enhancing effect of the M 23 C 6 -type carbides on the Vickers hardness. For the first time, this work revealed the evolution pathways of carbides within a Haynes® 282 superalloy prepared by WAAM, providing critical information for tunning the microstructure and mechanical properties. Finally, the carbide evolution kinetics established in this work can be potentially extended to other alloys prepared with WAAM, providing critical information to prevent mechanical failures associated with carbide coarsening.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Progression of creep deformation from grain boundaries to grain interior in Al-Cu-Mn-Zr alloys

Creep mechanisms are studied in θ'-Al 2 Cu-strengthened Al-Cu-Mn-Zr alloys at 300 and 350°C for (i) ACMZ, a base alloy without further alloying elements and (ii) RR350, a commercial alloy with additions of Ni and Co forming distinct grain-boundary precipitates. At high stresses, creep is dominated by dislocations bypassing θ' precipitates within grains via the Orowan mechanism, as evidenced by (i) very high stress exponent (n~20-25) and (ii) α-Al and θ' lattice strains (measured via in-situ neutron diffraction) evolving during creep in a manner consistent with load transfer from the plastically-deforming α-Al matrix to elastically-deforming θ' precipitates. At intermediate stresses, both alloys exhibit a n~3 regime, where α-Al and θ' lattice strains scale near-linearly with applied stress while remaining largely unaffected by strain accumulation, indicating that Orowan looping or dislocation pile-up around θ' is now inactive within the grains. Rather, dislocation motion occurs solely in θ'-precipitate-free zones (θ'-PFZ) where high dislocation densities are observed via TEM after creep deformation. Plastic flow at θ'-PFZ and/or localized pipe diffusion are expected to enable grain-boundary sliding (GBS), which is proposed as the rate-limiting mechanism in the n~3 regime. Ni/Co-rich precipitates at RR350 grain-boundaries, with negligible θ'-PFZ around them, share load (as determined via neutron diffraction) with the α-Al matrix more effectively than θ-Al 2 Cu precipitates at ACMZ grain-boundaries, with wide surrounding θ'-PFZ. So, high creep resistance in the n~3 GBS regime of RR350 is enabled by coarsening-resistant grain-boundary precipitates, forming without concomitant development of weak θ'-PFZ, which effectively share load with the grains.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microstructure Evolution of a Multimodal Gamma-Prime Ni-Based Superalloy Characterized by In Situ Diffraction

The relationship between the evolution of microstructure, deformation micromechanisms and mechanical properties is difficult to establish in multimodal size distribution $_γ$$'$ superalloys, as the microstructure evolves with both temperature and time, and multiple strengthening mechanisms across each size distribution contribute to mechanical performance. In situ X-ray scattering can offer unparalleled insight regarding microstructure evolution at the temperatures and stresses of importance to gas-turbine applications; however, in situ X-ray diffraction has not been applied to the study of multimodal $_γ$$'$ distribution superalloys. Herein, lattice parameter evolution of secondary and tertiary $_γ$$'$ precipitates in a representative superalloy, Nimonic 115, is determined between 750 °C and 950 °C and correlated to room-temperature SEM and microhardness values. A large positive lattice parameter misfit of secondary $_γ$$'$ induces precipitate splitting, and the tertiary $_γ$$'$ goes into dissolution at ~ 800 °C, but with little apparent change in hardness values. The volume fraction of $_γ$$'$ decreases above 900 °C and precipitate-matrix coherency is lost, and there is a corresponding decrease in microhardness values. Importantly, the diffraction analysis demonstrates the capability to determine critical microstructural parameters of both precipitate size distributions in situ, representing an additional tool for determining microstructure-mechanical property relationships of multimodal superalloys.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Effect of Thermal Aging on Microstructure and Stress Corrosion Cracking Behavior of an Alloy 152 1st Layer Butter Weldment

Nickel-based Alloy 690 and the associated weld Alloys 52 and 152 are typically used for nozzle penetrations in replacement heads for pressurized water reactor (PWR) vessels, because of their excellent overall resistance to general corrosion and environmental degradation, primarily stress corrosion cracking (SCC). However, many of the existing PWRs are expected to operate for 40- 80 years. Likewise, water-cooled small modular reactors (SMRs) will use Ni-Cr alloys and are expected to receive initial operating licenses for 60 years. Hence, the thermal stability of Ni-Cr alloys is critical for the long-term performance of both existing and advanced nuclear power plants, and possibly spent fuel storage containers. The objective of this research is to understand the microstructural changes occurring in high-Cr, Ni-based Alloy 152 weldments during long time exposure to the reactor operating temperatures, and the effect of these changes on the service performance. One area of particular concern is the potential for long range ordering (LRO), i.e. formation of the intermetallic Ni2Cr phase under prolonged exposure to reactor temperatures and/or irradiation, which can increase strength, decrease ductility, and cause dimensional changes or lead to in-service embrittlement of components made with these alloys. Hence, this research focused on the microstructural evolution and the SCC response of Alloy 152 under accelerated thermal aging. The materials studied involved three heats of Alloy 152 used to produce a dissimilar metal weld (DMW) joining an Alloy 690 plate to an Alloy 533 low alloy steel (LAS) plate, thermally aged at three different temperatures (370°C, 400°C and 450°C) for different durations up to 75,000h (equivalent to 60 years of reactor service). The microstructural characterization by means of synchrotron X-ray conducted in small, 0.2 mm - step line scans in the high-deformation regions of the weld root – covering areas spanning from the weld heat affected zone (HAZ) in Alloy 690 to the weld and weld butter on LAS - did not show evidence of LRO in any of the three Alloy 152 heats aged at 370°C and 450°C to an equivalent of 60 years of service. However, the first weld butter layer has high levels of deformation and is highly susceptible to SCC even in its non-aged condition. Nanohardness testing confirmed the extreme hardening with aging (ΔHV ≅ 100) at two locations within this weldment. In absence of LRO, hardening is suspected to be due to thermally-induced Cr carbide precipitation and coarsening. Testing in a primary water environment of the 1st layer of Alloy 152 weld butter aged at 370°C to a 60-year service equivalent revealed a fatigue and corrosion fatigue crack growth responses similar to those measured on the un-aged alloys. Similarly, the SCC CGR response of the aged weld butter does not appear to show a deterioration in performance, however, the difficult-to-test weldment geometry may affect the test results.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
NASA NTRS2004

Ar-Ar and I-Xe Ages and the Thermal History of IAB Meteorites

Studies of several samples of the large Caddo County IAB iron meteorite reveal andesitic material, enriched in Si, Nay Al and Ca, which is essentially unique among meteorites. This material is believed to have formed from a chondritic source by partial melting and to have further segregated by grain coarsening. Such an origin implies extended metamorphism of the IAB parent body. New Ar-39-Ar-40 ages for silicate from three different Caddo samples are consistent with a common age of 4.50- 4.51 Gyr ago. Less well defined Ar-Ar degassing ages for inclusions from two other IABs, EET8333 and Udei Station, are approx.4.32 Gyr, whereas the age for Campo del Cielo varies considerably over approx.3.23-4.56 Gyr. New I-129-Xe-129 ages for Caddo County and EET8333 are 4561.9 +/-0.1 Myr and 4560-4563 Myr, respectively, relative to an age of 4566 Myr for Shallowater. Considering all reported Ar-Ar ages for IABs and related winonaites, the range is approx.4.32-4.53 Gyr, but several IABs give similar Ar ages of 4.50-4.52 Gyr. We interpret these older ages to represent cooling after the time of last significant metamorphism on the parent body, and the younger ages to represent later Ar-40 diffusion loss. These older Ar-Ar ages are similar to Sm-Nd and Rb-Sr isochron ages reported in the literature for Caddo County. Considering the possibility that IAB parent body formation was followed by impact disruption, reassembly, and metamorphism (e.g., Benedix et al. 2000), the time of the post-assembly metamorphism may have been as late as approx.4.53 Gyr ago. However, precise I-Xe ages reported for some IABs define a range of ages of approx.4560 to approx.4576 My. The older I-Xe ages exceed the oldest precise radiometric ages of meteorites, appear unrealistic, and suggest a bias in the calibration of all I-Xe ages. But even with such a bias, the I-Xe ages of IABs cannot easily be reconciled with the much younger Ar-Ar and Sm-Nd ages and with cooling rates deduced from Ni concentration profiles in IAB metal (Herpfer et al., 1994). An explanation for the difference in radiometric ages of IABs may reside in combinations of the following: a) I-Xe ages have very high closure temperatures and were not reset during metamorphism; b) a bias exists in the K-40 decay constants; c) the reported Sm-Nd and Rb-Sr ages for Caddo are in error by amounts equal to or exceeding their reported 2-sigma uncertainties; and 4) the IAB parent body may have experienced a mild metamorphism approx.30 Myr after the initial heating that produced differentiation of Caddo silicate and mixing of silicate and metal. 129 129

Bogard, Donald D.↗
NASA NTRS2004

Ar-Ar and I-Xe Ages and the Thermal History of IAB Meteorites

Studies of several samples of the large Caddo County IAB iron meteorite reveal andesitic material, enriched in Si, Na, Al and Ca, which is essentially unique among meteorites. This material is believed to have formed from a chondritic source by partial melting and to have further segregated by grain coarsening. Such an origin implies extended metamorphism of the IAB parent body. New Ar-39-Ar-40 ages for silicate from three different Caddo samples are consistent with a common age of 4.50-4.51 Gyr ago. Less well defined Ar-Ar degassing ages for inclusions from two other IABs, EET8333 and Udei Station, are approx.4.32 Gyr, whereas the age for Campo del Cielo varies considerably over approx.3.23-4.56 Gyr. New I-129-Xe-129 ages for Caddo County and EET8333 are 4561.9+/-0.1 Myr and 4560- 4563 Myr, respectively, relative to an age of 4566 Myr for Shallowater. Considering all reported Ar-Ar ages for IABs and related winonaites, the range is approx.4.32-4.53 Gyr, but several IABs give similar Ar ages of 4.50-4.52 Gyr. We interpret these older ages to represent cooling after the time of last significant metamorphism on the parent body, and the younger ages to represent later Ar-40 diffusion loss. These older Ar-Ar ages are similar to Sm-Nd and Rb-Sr isochron ages reported in the literature for Caddo County. Considering the possibility that IAB parent body formation was followed by impact disruption, reassembly, and metamorphism (e.g., Benedix et al. 2000), the time of the post-assembly metamorphism may have been as late as approx.4.53 Gyr ago. However, precise I-Xe ages reported for some IABs define a range of ages of approx.4560 to approx.4576 Myr. The older I-Xe ages exceed the oldest precise radiometric ages of meteorites, appear unrealistic, and s,uggest a bias in the calibration of all I-Xe ages. But even with such a bias, the I-Xe ages of IABs cannot easily be reconciled with the much younger Ar-Ar and Sm-Nd ages and with cooling rates deduced from Ni concentration profiles in IAB metal (Herpfer et al., 1994). An explanation for the difference in radiometric ages of IABs may reside in combinations of the following: a) I-Xe ages have very high closure temperatures and were not reset during metamorphism; b) a bias exists in the K-40 decay constants; c) the reported Sm-Nd and Rb-Sr ages for Caddo are in error by amounts equal to or exceeding their reported 2-sigma uncertainties; and 4) the IAB parent body may have experienced a mild metamorphism approx.30 Myr after the initial heating that produced differentiation of Caddo silicate and mixing of silicate and metal.

Bogard, Donald D.↗
NASA NTRS2006

Ar-Ar and I-XE Ages and the Thermal History of IAB Meteorites

Studies of several samples of the large Caddo County IAB iron meteorite reveal andesitic material, enriched in Si, Na, Al and Ca which is essentially unique among meteorites. This material is believed to have formed from a chondritic source by partial melting and to have further segregated by grain coarsening. Such an origin implies extended metamorphism of the IAB parent body. New Ar-39- Ar-40 ages for silicate from three different Caddo samples are consistent with a common age of 4.50- 4.51 Gyr ago. Less well defined Ar-Ar degassing ages for inclusions from two other IABs, EET8333 and Udei Station, are approx. 4.32 Gyr, whereas the age for Campo del Cielo varies considerably over approx. 3.23-4.56 Gyr. New I-129-Xe-129 ges for Caddo County and EET8333 are 4561.9 plus or minus 0.1 Myr and 4560-4563 Myr, respectively, relative to an age of 4566 Myr for Shallowater. Considering all reported Ar-Ar ages for IABs and related winonaites, the range is approx. 4.32-4.53 Gyr, but several IABs give similar Ar ages of 4.50-4.52 Gyr. We interpret these older ages to represent cooling after the time of last significant metamorphism on the parent body, and the younger ages to represent later 40Ar diffusion loss. These older Ar-Ar ages are similar to Sm-Nd and Rb-Sr isochron ages reported in the literature for Caddo County. Considering the possibility that IAB parent body formation was followed by impact disruption, reassembly, and metamorphism (e.g., Benedix et al. 2000), the time of the postassembly metamorphism may have been as late as approx. 4.53 Gyr ago. However, precise I-Xe ages reported for some IABs define a range of ages of approx. 4560 to approx. 4576 Myr. The older I-Xe ages exceed the oldest precise radiometric ages of meteorites, appear unrealistic, and suggest a bias in the calibration of all I-Xe ages. But even with such a bias, the I-Xe ages of IABs cannot easily be reconciled with the much younger Ar-Ar and Sm-Nd ages and with cooling rates deduced from Ni concentration profiles in IAB metal (Herpfer et al., 1994). An explanation for the difference in radiometric ages of IABs may reside in combinations of the following: a) I-Xe ages have very high closure temperatures and were not reset during metamorphism; b) a bias exists in the K-40 decay constants; c) the reported Sm-Nd and Rb-Sr ages for Caddo are in error by amounts equal to or exceeding their reported 2-sigma uncertainties; and 4) the IAB parent body may have experienced a mild metamorphism approx.30 My after the initial heating that produced differentiation of Caddo silicate and mixing of silicate and metal.

Bogard, Donald D.↗
DOE OSTI2022

Predictive Tools for Customizing Heat Treatment of Additively Manufactured Aerospace Components

Laser-bed powder fusion (LBPF) additive manufacturing is increasingly being used to produce components of complex geometries using the Ni-base superalloy Inconel 718. The composition and the microstructure of the alloy are currently well optimized for wrought components made using conventional manufacturing processes such as rolling, forging, extrusion, etc. The attractive mechanical properties of the alloy result from the underlying austenitic matrix with fine equiaxed grains, and a high density and uniform distribution of the precipitation hardening phase, γ". Heat treatment steps such as homogenization, solutioning and aging are well documented for the wrought alloy. However, when the same wrought alloy compositions are used for the additive manufacturing (AM) processes, the asprocessed microstructure is significantly different, because of the different thermal history associated with LBPF, including rapid solidification and multiple temperature excursions that lead to multiple re-melting and reheating in the solid state. Rapid solidification introduces potential non-equilibrium effects at the moving solid-liquid interfaces that impact the extent of solute segregation, as well as the morphology of the dendritic grains that form. In order to recover the target mechanical properties, AM components have to undergo post-process heat treatments. However, such heat treatments have to be custom designed for the AM process and the component geometry because of the expected vast differences in the microstructure at various locations of a component with complex geometry. The homogenization and precipitation steps should be optimized for the component so that target mechanical properties can be obtained throughout the part. The objective of this research is to utilize High Performance Computing in phase field simulations of microstructure evolution during post-processing of AM components. The physics-based modeling will be beneficial in reducing the experimental effort required for heat treatment process selection, optimization, and certification, thus leading to a significant reduction in energy consumption for AM and post-processing heat treatment. The optimization study will help identify heat treatments steps that are critical for development of a final desired microstructure with the minimum energy input. This combined with shortening of the production cycle (time-to-market) by reducing the number of failed parts (property targets), and reduction in the number of iterations for process optimization, will enable 30-40% savings in the energy costs. Phase field simulations of the degree of homogenization and the effect of local matrix composition on the nucleation and growth of competing precipitating phases were performed using the Microstructure Evolution Using Massively Parallel Phase Field Simulations code developed in-house at the Oak Ridge National Laboratory. The simulations were able to successfully capture the kinetics of nucleation and growth, and morphologies of various precipitating phases as a function of local matrix compositions and composition gradients characteristic of local microstructures arising from location-dependent variations in the thermal conditions. Future work will involve extending the simulations to a length scale consisting of multiple dendrites, so that the effect of homogenization on the coarsening of the dendrites can be simulated and used as an additional input to the optimization of the heat treatment process.

36 MATERIALS SCIENCE↗