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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Sigma phase evolution and nucleation mechanisms revealed by atom probe tomography in a 347H stainless steel

The size evolution and phase composition of sigma phases were investigated for a 347H stainless steel subject to isothermal aging at 750 °C for up to 10,000 h. Scanning electron microscopy reveals that sigma phases are present before 336 h aging and they continue to grow for all aging times studied. Atom probe tomography shows little variation in the sigma phase composition with aging time up to 10,000 h, and only the C content decreases with aging time. The comparison of C concentration suggests that the sigma phase does not nucleate within the C-depleted matrix or precipitate free grain boundaries, leaving dissolving metastable M 23 C 6 as the only possible nucleation site. Based on the experimental results and thermodynamic simulations, the desirable Nb concentration is discussed to reduce the kinetics of sigma phase growth, and possible design directions are suggested to improve 347H.

36 MATERIALS SCIENCE↗
NASA NTRS1974

Effects of sigma-phase formation on some mechanical properties of a wrought nickel-base superalloy (IN-100)

The effect of sigma phase formation on an extruded and forged nickel base superalloy with the composition of the casting alloy IN-100 was studied. By adding only aluminum and titanium to remelt stock, three compositions were produced which had varying propensities for sigma formation. These compositions were given a four step heat treatment and were stress-ruptured or tensile tested. The very sigma prone composition had a shorter rupture life than the sigma-free or moderately sigma prone compositions when tested at 843 and 885 C. Elongation in room temperature tensile tests was considerably lower for the very sigma prone composition than for the other two wrought compositions after prolonged exposure at 732 or 843 C.

Dreshfield, R. L.↗
NASA NTRS1993

Predicting Formation Of Sigma Phase In Alloys

SUPER PHACOMP developed after research into many versions of PHACOMP algorithm. Resulting program implements three of these versions, enabling comparison of results to give greater reliability to predictions. Inasmuch as certain calculations common to each, three versions woven together for efficiency. While prediction of formation of sigma phase is primary function, also performs other calculations of properties of alloys. Program benefits anyone working in design of alloys. Written in BASIC.

Kaukler, William F.↗
DOE OSTI2020

Study on the continuous phase evolution and physical properties of gas-atomized high-entropy alloy powders

In this study, AlCoCrFeNi high entropy alloy (HEA) powders were fabricated by gas atomization process, and the effects of annealing heat treatment on phase evolution and mechanical properties were investigated. The as-atomized powders have pure BCC phase with a spherical shape and equal composition distribution, and then the FCC and sigma phase sequentially generated after annealing. The mechanical property such as hardness was evidently enhanced, which was caused by precipitation hardening effect. After the raw powders were annealed at 600 °C, the FCC (Al–Ni) phase began to precipitate, the its phase intensity raised with the annealing temperature. Then, the sigma phase (Fe– Cr)formed as the annealing temperature reached 800 °C. Both mechanical properties and lattice constant were influenced by heating effect. According to the results, the lattice became loose with the increasing temperature. In summary, the mechanical properties and phase constitutions of gasatomized AlCoCrFeNi HEA powders can be adjusted via annealing process, resulting in precipitation hardening effect.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2025

CALPHAD-based Bayesian optimization to accelerate alloy discovery for high-temperature applications

Two crucial properties influencing the performance of high-temperature alloys are coefficient of thermal expansion (CTE) and phase constitution. It is desirable to have alloys with low CTE, which reduces CTE mismatch with the surface oxide and the likelihood of oxide spallation. Reducing the amount of brittle intermetallic phases such as Sigma (σ) enhances alloy ductility and processability. Here, we propose a multi-objective Bayesian Optimization (BO) model to simultaneously minimize CTE (at an operational temperature of 1150 °C) and T σ (temperature when the Sigma phase completely dissolves in the metal matrix), properties which are obtained from high-throughput CALculation of PHAse Diagrams (CALPHAD). The model successfully identifies several alloys with CTE ≤ 2 × 10 –5 /K and T σ ≤ 500 °C by exploring just 7% of the nickel–chromium–cobalt–aluminum–iron (Ni–Cr–Co–Al–Fe) composition space. Such multi-objective alloy design frameworks can be used to inform additive manufacturing experiments and accelerate alloy discovery for high-temperature energy applications.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microstructure-Based Understanding of High-Temperature Deformation Behaviors in Laser Powder Bed Fusion (LPBF) 316H Stainless Steel

This report presents the results of high-temperature mechanical property testing and microstructural analysis of laser powder bed fusion (LPBF) 316H stainless steel (SS) conducted during Fiscal Year 2025 (FY25) under the U.S. Department of Energy, Office of Nuclear Energy’s Advanced Materials and Manufacturing Technologies (AMMT) program. The study builds upon prior work by expanding the mechanical property test matrix and advancing a microstructure-based mechanistic understanding of LPBF 316H SS performance, with a focus on the solution annealed (SA, 1100°C for 1 hour) materials. High-temperature tension, creep, fatigue, and creep-fatigue tests were performed. Thermal aging studies were conducted. Advanced characterization techniques, including scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), and high-energy synchrotron X-ray diffraction, were employed to investigate the microstructural evolution during thermal aging and mechanical testing. It was discovered that the as-built (AB) LPBF 316H SS exhibited precipitation kinetics during thermal aging that are 10–100 times faster than its wrought counterpart due to the presence of high densities of preferred nucleation sites, while the precipitation kinetics in SA LPBF 316H was under investigation. The accelerated precipitation of embrittling phases such as sigma phase in LPBF 316H SS compared to its wrought counterpart led to significant impacts on creep ductility. The influence of laser printing parameters and build orientations on fatigue and creep-fatigue performance was observed. In assessing the creep-fatigue performance, it was discovered that the SA LPBF 316H samples failed in less than 200 cycles under 595°C, 0.5% (strain amplitude) with a 60-minute hold time. This work establishes a mechanistic framework for predicting the long-term behavior of LPBF 316H SS, supporting its rapid qualification under the ASME BPVC. The findings contribute to the broader goal of enabling the deployment of advanced materials in next-generation nuclear energy systems. An outlook for FY26 work, including continued aging studies, mechanical testing, and microstructural characterization, is provided.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Computational thermodynamics-guided alloy design and phase stability in CoCrFeMnNi-based medium-and high-entropy alloys: An experimental-theoretical study

A computational thermodynamics approach has been employed to design CoCrFeMnNi-based medium- and high-entropy alloys (M/HEAs) with systematically varied compositions (Co(( 80-X )/ 2 )Cr(( 80-X )/ 2 )Fe X Mn 10 Ni 10 with x = 30, 40, and 50 at.%) and phase stability. Since the formation of sigma phase, usually brittle and undesirable, is a common concern, when this class of alloys is subjected to elevated temperatures (600–1000 °C), predicting its formation becomes essential. Thus, its formation and the phase equilibria were studied using the CALPHAD method, and two empirical methods, namely, valence electron concentration (VEC) and paired sigma-forming element (PSFE). Isothermal aging treatments at 900–1100 °C for 20 h were performed, since CALPHAD and VEC/PSFE predictions diverged. Both prediction methods were compared with experimental characterization by a combination of scanning electron microscopy and high-energy synchrotron X-ray diffraction. In conclusion, the predictions from the VEC/PSFE and CALPHAD calculations (depending on the database used) were shown to be quite accurate.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Characterization of Precipitation-Strengthening Heat-Resistant Austenitic Stainless Steels for Life-Prediction Modeling

In this study, the role of minor alloying additions in 347H stainless steels (UNS34709, ASTM A240/240M) on creep-rupture properties at 650-750°C and microstructure evolution during isothermal exposure at 750°C has been investigated, aiming to provide the experimental dataset as boundary conditions of physics-based modeling for material/component life prediction. Four different 347H heats containing various amounts of boron and nitrogen additions were prepared and evaluated. The combined additions of B and N are found to stabilize the strengthening secondary M23C6 carbides and retarding the transition from M23C6 to sigma phase precipitates during thermal exposure. The observed kinetics of microstructure evolution reasonably explains the improvement of creep-rupture properties of 347H stainless steels with the B and N additions.

Yamamoto, Yukinori↗
DOE OSTI2021

Elemental segregation to lattice defects in the CrMnFeCoNi high-entropy alloy during high temperature exposures

The influence of small plastic pre-strains on the elevated-temperature stability and microstructure of the equiatomic CrMnFeCoNi FCC solid solution is investigated. Particular attention is given to whether any of the alloy elements segregate to individual dislocations. To that end, CrMnFeCoNi samples were first deformed in tension at room temperature to plastic strains of 0.2 and 2.3%, and subsequently annealed at 973 K for 800 hours. The pre-strains activated planar slip of 1/2<110>-type dislocations on {111}-type glide planes. Interactions of this planar slip with special Σ3 grain boundaries formed a large number of dislocation segments with a <110>-type crystallographic orientation suitable for a credible end-on analysis of dislocation cores in HR-STEM. The cores of the 1/2<110> dislocations pushed up against the investigated grain boundaries were found to be close to the compact configuration. Within the sensitivity of the Super-X EDS mapping, no concentration gradient was detected near dislocations that would indicate enrichment at dislocation cores of any of the elemental constituents of the alloy after the pre-deformation and annealing. However, a Cr-rich tetragonal sigma phase nucleated and grew at grain boundary triple junctions during this anneal, processes that were not accelerated by the enhanced dislocation density present after pre-strain. A clear chromium gradient was observed in the Cr-depleted zones near grain boundaries suggesting that Cr transport occurred by relatively slow diffusion from the bulk to the grain boundaries and then by relatively fast diffusion along the grain boundaries to the precipitates. Accompanying the Cr depletion near grain boundaries is a simultaneous Ni and Mn enrichment, which promotes formation of the L1 0 NiMn phase that is observed on the grain boundaries after prolonged annealing.

36 MATERIALS SCIENCE↗
NASA NTRS1987

Defects in nickel-base superalloys

The presence of substantial amounts of the sigma phase in Ni-base superalloys can drastically reduce the alloy's stress rupture life. No predictive system exists which is entirely successful in anticipating the formation of sigma, mu, and similar phases in new and substantially different alloys. Freckles are defects due to the segregation of elements in quantities that can lead to phase precipitation, and are caused by gravity-driven fluid motion that yields microsegregation in the ingots typically used in the fabrication of structures based on these alloys. Also noted are the effects of porosity and grain boundaries on superalloy mechanical properties.

Dreshfield, Robert L.↗
DOE OSTI2024

Additively manufactured Ni-20Cr to V functionally graded material: Computational predictions and experimental verification of phase formations

Throughout this work, a database for the Cr-Ni-V system was constructed by modeling the binary Cr-V and ternary Cr-Ni-V systems using the CALPHAD approach aided by density functional theory (DFT)-based first-principles calculations and ab initio molecular dynamics (AIMD) simulations. To validate this new database, a functionally graded material (FGM) using Ni-20Cr and elemental V was fabricated using directed energy deposition additive manufacturing (DED AM) and experimentally characterized. The deposited Ni-20Cr was pure fcc phase, while increasing the amount of V across the gradient resulted in the formation of sigma phase, followed by the bcc phase. The experimentally measured phase data was compared with computational predictions made using a Cr-Ni-V thermodynamic database from the literature as well as the database developed in the present work. The newly developed database was shown to better predict the experimentally observed phases due to its accurate modeling of binary systems within the database and the ternary liquid phase, which is critical for accurate Scheil calculations.

36 MATERIALS SCIENCE↗
NASA NTRS1982

Effect of reduced cobalt contents on hot isostatically pressed powder metallurgy U-700 alloys

The effect of reducing the cobalt content of prealloyed powders of UDIMET 700 (U-700) alloys to 12.7, 8.6, 4.3, and 0% was examined. The powders were hot isostatically pressed into billets, which were given heat treatments appropriate for turbine disks, namely partial solutioning at temperatures below the gamma prime solvus and four step aging treatments. Chemical analyses, metallographic examinations, and X-ray diffraction measurements were performed on the materials. Minor effects on gamma prime content and on room temperature and 650 C tensile properties were observed. Creep rupture lives at 650 C reached a maximum at the 8.4% concentration, while at 760 C a maximum in life was reached at the 4.3% cobalt level. Minimum creep rates increased with decreasing cobalt content at both test temperatures. Extended exposures at 760 and 815 C resulted in decreased tensile strengths and rupture lives for all alloys. Evidence of sigma phase formation was also found.

Harf, F. H.↗
NASA NTRS1983

Metallurgical studies of NITRONIC 40 with reference to its use for cryogenic wind tunnel models

The characterstics of NITRONIC 40 were investigated in connection with its use in cryogenic wind tunnel models. In particular, the effects of carbide and sigma-phase precipitation resulting from heat treatment and the presence of delta ferrite were evaluated in relation to their effects on mechanical properties and the potential consequences of such degradation. Methods were examined for desensitizing the material and for possible removal of delta ferrite as a means of restoring the material to its advertised properties. It was found that heat treatment followed by cryogenic quenching is a technique capable of desensitizing NITRONIC 40. However, it was concluded that it is extremely difficult, if not impossible, to remove the delta ferrite from the existing stock of material. Furthermore, heat treatments for removing delta ferrite have to take place at temperatures that cause very large grain growth. The implications of using the degraded NITRONIC 40 material for cryogenic model testing were reviewed, and recommendations were submitted with regard to the acceptability of the material. The experience gained from the study of NITRONIC 40 clearly identifies the need to implement a policy for purchasing top-quality materials for cryogenic wind tunnel model applications.

Wigley, D. A.↗