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At least 19 records

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↗

Microstructure and Temperature Dependent Indentation Response of Additively Manufactured Precipitation-Strengthened Al 0.3 Ti 0.2 Co 0.7 CrFeNi 1.7 High Entropy Alloy

The temperature-dependent [from room temperature (RT) to 500°C] nanoindentation behavior of a precipitation-strengthened Al 0.3 Ti 0.2 Co 0.7 CrFeNi 1.7 high-entropy alloy (HEA) processed via two different additive manufacturing (AM) techniques was investigated in the as-deposited and annealed conditions. The hierarchically heterogeneous microstructures were achieved via simple one-step annealing treatments, exploiting the residual stresses in the AM-processed HEA to partially recrystallize the microstructure, performed remarkably better than the nearly homogeneous microstructures in the as-deposited state. Further, the one-step annealed conditions revealed < 6.6% reduction in hardness values at 500°C compared to RT, while the as-deposited conditions showed a > 18% reduction in the hardness. The one-step annealed conditions also exhibited significantly higher hardness than the as-deposited conditions owing to their L1 2 -strengthened FCC microstructures. Furthermore, serrated yielding or the Portevin-Le Chatlier effect indicative of microstructural instability was observed during nanoindentation deformation (at 500°C) for the as-deposited conditions but not for the one-step annealed conditions. This, therefore, signifies the robustness of the hierarchically heterogeneous microstructures at elevated temperatures presenting a strong avenue for tuning the HEAs for future nuclear reactor applications.

36 MATERIALS SCIENCE↗

Hardenability and microstructural evolution of a precipitation strengthened Ni 50 Ti 21 Hf 25 Al 4 alloy

NiTi-based quaternary alloys are used in a variety of mechanical components, such as bearings, actuators, and dampers, owing to their good hardenability, wear resistance, and corrosion resistance. Additionally, one of the most notable characteristics of NiTi-based alloys is their shape memory effect and pseudoelastic properties. Connecting the macroscopic processing parameters employed in the design of new intermetallic alloys to the nanoscale structural characteristics dictating their behavior is crucial for improving their mechanical properties and expanding the spectrum of potential applications. Here, in this work, an arc melted Ni 50 Ti 21 Hf 25 Al 4 (at%) alloy was solution treated at 1050 °C followed by quenching and aging at 600 °C to investigate the effect of aging time on the microstructure and mechanical properties. Two types of nano-sized precipitates were observed and determined as face-centered orthorhombic H-phase (TiHf)Ni and L2 1 Heusler precipitates Ni 2 TiAl. The morphology and orientation of the H-phase were investigated using scanning and transmission electron microscopy (SEM and TEM), elucidating the coarsening kinetics and strengthening contribution of that phase to the intermetallic mechanical behavior. Following coarsening, the presence of Heusler nanoprecipitates was detected under overaged conditions through TEM imaging and nanobeam electron diffraction patterns. A peak hardness condition of 756 HV was achieved after 70 h of aging, indicating that the co-precipitation of H-phase and Heusler precipitates through a well-designed aging treatment can lead to optimal mechanical performance, thus elevating the alloy’s potential as a viable material for industrial applications.

36 MATERIALS SCIENCE↗

Using post-processing heat treatments to elucidate precipitate strengthening of additively manufactured superalloy 718

The poor machinability and extensive work hardening of Ni-based superalloys makes additive manufacturing an attractive option for producing geometrically complex components with distinct microstructures. Although previous studies show recovery of high strength at room temperature, very few studies demonstrate successful properties at elevated temperatures required for industrial applications. Here, the objectives of this study are to present a post-build heat treatment for high strength across a wide temperature range, determine the strength contribution of nanoscale precipitating phases to the overall mechanical properties of superalloy 718, and from these, provide a comprehensive microstructure-property relationship for wrought and AM 718 to guide efforts to simulate the properties of AM components. Laser powder bed fusion–produced superalloy 718 was characterized at multiple length scales using scanning electron microscopy and transmission electron microscopy in the as-built condition and with multiple heat treatments designed to form combinations of γ', γ", and δ precipitates. Uniaxial tensile tests performed from room temperature to 600 °C on subsize specimens determined the yield strength, elastic modulus, ultimate tensile strength, fracture stress, and uniform elongation. Precipitates in this work proved to be weak barriers to dislocation motion through a dispersed barrier model, but they provided strength to the alloy through their consistent high density. The relative contribution to the yield strength from γ" remained consistent between 48% and 57% of the total strength up to 600 °C, the primary influence on the high temperature strength of superalloy 718. The strength factors for γ" and δ precipitates were found to trend inversely with tensile test temperature and may be attributable to the differences in precipitate coherency. A post-build heat treatment is recommended to maintain high strength at elevated temperatures. A quantitative microstructure-property relationship, dependent on precipitate size, density, and morphology, was derived and can estimate the yield strength across a wide temperature range applicable to the operational regimes for superalloy 718.

36 MATERIALS SCIENCE↗

Rapid Design of Cost-Effective Refractory High Entropy Alloys Strengthened by Precipitation

Funded by the ARPA-E ULTIMATE program, this project aims to develop cost-effective refractory high entropy alloys (RHEAs) for gas turbine blades applications at 1300 degree Celsius and above. The alloy design focuses on carbides precipitation strengthening in a strong and ductile solid solution BCC matrix. The goal is to achieve balanced mechanical properties including room temperature ductility & fracture toughness and high temperature strength and creep resistance, while maintaining comparable oxidation resistance and densities to Ni-base superalloys. To accelerate alloy design, multiscale modeling including CALPHAD and first-principles density functional theory (DFT) calculations and machine learning are performed. Specifically, high throughput phase diagram calculations and screening are carried out using CALPHAD; DFT calculations are performed to predict intrinsic ductility, grain boundary strengthening potential, coefficient of thermal expansion (CTE) and temperature-dependent elastic constants. Temperature dependent yield stress, creep strain and CTE are also predicted using machine learning. Down-selected alloys are synthesized in small buttons of about 250g using arc melting for rapid evaluation on microstructure and mechanical properties before employing plasma arc melting and additive manufacturing for producing large ingots. Preliminary computational and experimental results of this project will be presented and future direction in RHEA development will be discussed.

high temperature materials↗

Rapid Design and Manufacturing of High-Performance Materials for Turbine Blades

This research demonstrated the concept of carbide precipitation-strengthened refractory high entropy alloys (RHEA). The advantage of a precipitation strengthened alloy is all phases are in thermodynamic equilibrium promoting microstructural stability, and consequently retention of properties at elevated temperatures. Additionally, as with any precipitation strengthened – or age hardened - alloy, components can be heat-treated after manufacturing to manipulate the microstructure and optimize properties for performance. This is an advantage of the precipitation strengthened alloys over composites and ceramics materials, where the microstructure and properties are essentially fixed upon the initial materials manufacturing stage. High throughput (HT), multi-scale computer modeling was used to identifying novel RHEA compositions with desired characteristics needed for precipitation strengthening. Designs were validated by producing small ingots via are melting. The results showed that carbides precipitated and consequently, the strength of the alloys (measured in compression) increased after heat-treatment, which is the desired effect. The project also demonstrated the feasibility of producing articles from RHEA by additive manufacturing (AM). Electron beam melting (EBM) and laser direct energy deposition (L-DED) additive manufacturing methods, were explored with various processing parameters were interrogated for both methods. Sound (crack-free and dense) precipitation strengthened RHEA samples were produced via EDM AM, demonstrating the feasibility of the concept.

36 MATERIALS SCIENCE↗

Final Scientific/Technical Report Rapid Design and Manufacturing of High-Performance Materials for Turbine Blades

This research demonstrated the concept of carbide precipitation-strengthened refractory high entropy alloys (RHEA). The advantage of a precipitation strengthened alloy is all phases are in thermodynamic equilibrium promoting microstructural stability, and consequently retention of properties at elevated temperatures. Additionally, as with any precipitation strengthened – or age hardened alloy, components can be heat-treated after manufacturing to manipulate the microstructure and optimize properties for performance. This is an advantage of the precipitation strengthened alloys over composites and ceramics materials, where the microstructure and properties are essentially fixed upon the initial materials manufacturing stage. High throughput (HT), multi-scale computer modeling was used to identifying novel RHEA compositions with desired characteristics needed for precipitation strengthening. The results showed that carbides precipitated and consequently, the strength of the alloys (measured in compression) increased after heat-treatment, which is the desired effect. The project also demonstrated the feasibility of producing articles from RHEA by additive manufacturing (AM).

36 MATERIALS SCIENCE↗

Improved creep performance of CoCrFeNi high entropy alloys by Mo addition

The CoCrFeNi family of high entropy alloys has good mechanical and corrosion properties, performing like stainless steels with low yield stresses. They could, however, benefit from hardening methods for structural and high temperature applications. Here, this work investigates the potential for the CoCrFeNi alloy to be hardened with the addition of Mo. A series of CoCrFeNiMo alloys and their CoCrFeNi counterparts were subsequently manufactured at NETL and then mechanically creep tested at 650°C. The alloys were designed to possess a range of stacking fault energies which influence the mechanical properties of the alloys via the motion of their dislocations under stress. Results show that Mo-containing variants have creep rupture lives ranging from 4000 to 8000 hours, i.e., about two orders of magnitude longer than those for Mo-free variants. The significantly improved creep performance of the Mo-containing alloys is due to a combination of solid solution strengthening and precipitation strengthening from µ-phase and carbides.

36 MATERIALS SCIENCE↗

Gaseous Hydrogen Embrittlement of L-PBF Ni-Based Superalloys for Service in Natural Gas Turbines

Efforts to improve efficiency of industrial gas turbine engines have focused on increasing operating temperatures by use of fuel-flexible gas blends. Ni-based superalloys are susceptible to hydrogen embrittlement (HE), leading to potential risk of premature component failure. Certain turbine components exposed to hydrogen-rich environments are manufactured from additive processes like laser powder bed fusion (L-PBF). The HE susceptibility was evaluated for three Ni-based superalloys: solid solution strengthened Alloy 625, γ’/γ’’-precipitation strengthened Alloy 718, and γ’-precipitation strengthened Haynes® 282®. L-PBF samples were pre-charged under medium and high pressure gaseous hydrogen before tensile testing at temperatures up to 260 °C using a fast strain rate. Selected samples were subjected to a service conditioning heat treatment prior to hydrogen charging to evaluate the change in susceptibility after prolonged service. The susceptibility to HE and HE mechanisms of these three alloys is compared.

additive manufacturing↗

Microstructural evaluation of the creep behavior in L-PBF Ni-based superalloys

This presentation at ICAM 2024 Conference focuses on the commonalities and differences in the creep rupture behavior and creep mechanisms for three distinct classes of laser powder-bed fusion (L-PBF) Ni-based superalloys (γ’-precipitate strengthened Haynes® 282®, γ’/γ”/δ-precipitate strengthened Alloy 718, and solid-solution strengthened Alloy 625) as compared to conventionally processed counterparts. A comparison of Larson-Miller parameter plots establishes that these alloys perform statistically within the bounds established for the wrought product, despite having dissimilar microstructural features and other artefacts associated with PBF-LB manufacturing and post-processing heat treatment. To understand the failure and the impact of composition, minor phases, and deformation defects on creep behavior, the fractography has been performed and microstructures have been evaluated in detail with SEM-EDS, EBSD, and HAADF-STEM. The underlying diffusional and dislocation creep mechanisms associated with this microstructural evaluation is discussed. This work is supported by NETL-FWP-1022408 Advanced Turbines.

Sudbrack, Chantal↗

Rapid assessment of interfacial stabilization mechanisms of metastable precipitates to accelerate high-temperature Al-alloy development

Precipitate strengthened high-temperature alloys are currently used in safety-critical applications. Understanding precipitate stability and solute segregation mechanisms at high temperatures is key to designing high-strength alloys. Rapid in-situ approaches, therefore, are pivotal in accelerating the alloy design process. Hereby using the test case of a promising high-temperature Al-Cu-Mn-Zr alloy, we demonstrate the value of in-situ atom probe tomography coupled with in-situ transmission electron microscopy to reveal atomic-scale mechanisms that lead to the emergence of non-equilibrium solute segregation. Mn and Zr segregation at strengthening precipitate(θ’)-matrix interface increases the kinetic barrier for phase transformation thus retaining high-temperature strength.

36 MATERIALS SCIENCE↗

Solidification behavior and cracking mechanisms of Ru-containing BCC-B2 superalloys

Many precipitation-strengthened alloys are highly susceptible to cracking during additive manufacturing (AM), which often requires compositional adjustments to mitigate. Recently, it has been demonstrated that refractory BCC alloys can be precipitation strengthened with ordered Ru-containing B2 precipitates to temperatures exceeding 1200 °C. This motivates a study of the potential fabricability of quaternary and quinary refractory BCC-B2 alloys by AM using single track laser experiments. Alloys with greater than 9 at.% Ru exhibit crack formation upon cooling. Solidification cracking was observed in all Zr-containing alloys, which can be mitigated by substituting Hf. Furthermore, this cracking is attributed to the strong partitioning of Zr during solidification, as revealed by characterization of alloy solidus, liquidus, and partition coefficients. Hf 5 Ru 4 -Nb 63 V 28 is identified as a promising BCC-B2 composition with a high B2 solvus (>1300 °C) and solidus (1695 °C) along with a high resistance to cracking.

36 MATERIALS SCIENCE↗

The role of cellular structure, non-equilibrium eutectic phases and precipitates on quasi-static strengthening mechanisms of as-built AlSi10Mg parts 3D printed via laser powder bed fusion

The quasi-static loading strengthening mechanism in the as-built state of an AlSi10Mg alloy 3D-printed via Laser Powder Bed Fusion (LPBF) was thoroughly identified and quantified using state-of-the-art electron microscopy and synchrotron X-ray diffraction techniques. The yield strength was comprehensively modelled through an in-depth characterization and quantification of the microstructural features as well as their effective volumes for strengthening. In particular, the non-equilibrium eutectic network was characterized with a two-fold structure: cell boundary particles as well as intracellular lamellar/fibrous networks, each consisting of discrete phases exhibiting a thru-thickness compositional gradient, a semi-coherent interface with the matrix and an abundance of crystal defects such as nano-sized sub-grains, microstrains and stacking faults. Further, these altogether made the eutectic phase the most potent contributor to the yield strength accounting for ~30–40% of the estimated value (i.e., cell boundary and eutectic network strengthening combined). Precipitates strengthening was identified as the second most potent mechanism via a shearing process only. Moreover, the presented methodology was able to capture the effect of LPBF processing variables on the individual strengthening contributions, e.g., the effect of a lower laser scanning speed on increasing the cell size as well as the mean precipitate size, which are shown to exhibit opposing impacts on strengthening.

36 MATERIALS SCIENCE↗

Dual-precipitates enhance fatigue resistance in an additively manufactured high-entropy alloy

To accomplish the intense desire of high-strength materials for enhanced energy-efficiency, recent research applies a combined strategy of additive-manufacturing and precipitation-strengthening in high entropy alloys. In a context, Al 0.2 Co 1.5 CrFeNi 1.5 Ti 0.3 nanoprecipitation-strengthened system was developed, demonstrating very convincing strength and toughness. Moreover, additive-manufacturing facilitated additional strength by well-decorated cell-boundaries with blocky L2 1 precipitates and homogeneously distributed L1 2 precipitates. However, fatigue research of this alloy remained unexplored despite being the main precursor for structural applications. In this study low-cycle fatigue behavior of this alloy in both as-built and precipitation-strengthened (aged) conditions has been explored, combined with in-situ neutron diffraction investigation. Findings revealed a substantial cyclic-stress profile and a notable fatigue-life below ±0.50% strain-amplitude, exceeding 10 5 cycles at ±0.30% strain-amplitude. These demonstrate the potential to carry higher payloads with marked engineering-reliability. Residual-stress estimation revealed strain-compatibility between the matrix and L1 2 precipitate, indicating a crack-initiation immune interface. A comparative examination of dislocation character revealed shifting towards pure edge-character in aged alloy indicates precipitates promoted planar-slip during deformation.

36 MATERIALS SCIENCE↗

Fabrication and Testing of Solid-Solution Strengthened Corrosion Resistant Alloys For Service in Molten Fluoride Environments

The demand for higher system thermal efficiencies requires the operation of power generation cycles and heat conversion systems at progressively higher temperatures. As the system operating temperature increases, existing materials may not provide adequate mechanical properties or environmental compatibility or both. There is an increasing commercial interest in the development and deployment of liquid-fueled Molten Salt Reactors (MSRs). Hastelloy®N, the highest performing candidate MSR structural alloy, is not capable of operations at temperatures above 700°C, thus limiting the performance of these systems. Using an Integrated Computational Materials Engineering (ICME)-approach and small laboratory scale heats, ORNL developed a class of patented alloys covered by U.S. Patent 9, 435, 011 B2, “Creep-resistant, Cobalt-free alloys for high temperature, liquid-salt heat exchanger systems,” similar to Hastelloy®N in that they are primarily solid solution strengthened. In contrast to precipitation strengthened alloys, the microstructure of solid solution alloys and hence the high temperature mechanical properties are stable for extended periods of time allowing long reactor operating life. The new alloys have shown to possess good resistance to liquid fluorides at temperatures up to 850°C and have significantly improved creep properties when compared to Hastelloy®N. The purpose of the CRADA project was for ORNL to collaborate with Haynes International- a materials producer, MetalTek International- a foundry, and Kairos Power – an advanced reactor developer – to scale-up selected alloys, evaluate their properties, and identify one solid solution strengthened alloy that can meet the property requirements for the reactor being developed by Kairos Power and other similar liquid fluoride-salt cooled reactors. As part of the project, eight alloys were down-selected and fabricated in larger industrial scale heats by Haynes International. Resistance to molten salt was evaluated in flowing FLiNaK and FLiBe by Kairos Power using their Rotating Cage Loop (RCL) system. Accounting for iron deposition during these tests, the new alloys displayed very low net mass change showing excellent corrosion performance in molten salt. Creep properties evaluated at ORNL were found to be better than that of Hastelloy®N and 316 stainless steel. Long-term stabilities of the alloys evaluated by Haynes International showed that these alloys have excellent thermal stability in the temperature range 704.4-815.6°C, with the change in strength and ductility being less than 10-15% after a 4000-hour exposure at 815.6°C. Autogenously Gas Tungsten Arc Welding (GTAW) welded samples showed less than 10% change in yield strength / ultimate tensile strength / total elongation compared to the basemetal, indicating that the alloys have excellent weldability. Three parts were successfully investment-cast using one alloy with very little voiding showing feasibility of fabricating parts using the casting process. This project enabled extensive interaction between the material producer Haynes International, casting supplier MetalTek, and reactor developer Kairos Power. This facilitated testing of materials and components produced using the newly developed alloys by the end-user. This allowed the generation of critical dataset required for down-selection of a few promising alloys for further development. This data is also currently being shared with other reactor designers for them to evaluate the suitability of this alloy for their reactor design. The availability of this alloy will ultimately enable the design and development and deployment of MSRs with increased temperature of operation and thus, improved efficiencies.

99 GENERAL AND MISCELLANEOUS↗

Fabrication and Testing of Solid-Solution Strengthened Corrosion Resistant Alloys For Service in Molten Fluoride Environments

The demand for higher system thermal efficiencies requires the operation of power generation cycles and heat conversion systems at progressively higher temperatures. As the system operating temperature increases, existing materials may not provide adequate mechanical properties or environmental compatibility or both. There is an increasing commercial interest in the development and deployment of liquid-fueled Molten Salt Reactors (MSRs). Hastelloy®N, the highest performing candidate MSR structural alloy, is not capable of operations at temperatures above 700°C, thus limiting the performance of these systems. Using an Integrated Computational Materials Engineering (ICME)-approach and small laboratory scale heats, ORNL developed a class of patented alloys covered by U.S. Patent 9,435,011 B2, “Creep-resistant, Cobalt-free alloys for high temperature, liquid-salt heat exchanger systems,” similar to Hastelloy®N in that they are primarily solid solution strengthened. In contrast to precipitation strengthened alloys, the microstructure of solid solution alloys and hence the high temperature mechanical properties are stable for extended periods of time allowing long reactor operating life. The new alloys have shown to possess good resistance to liquid fluorides at temperatures up to 850°C and have significantly improved creep properties when compared to Hastelloy®N. The purpose of the CRADA project was for ORNL to collaborate with Haynes International- a materials producer, MetalTek International- a foundry, and Kairos Power – an advanced reactor developer – to scale-up selected alloys, evaluate their properties, and identify one solid solution strengthened alloy that can meet the property requirements for the reactor being developed by Kairos Power and other similar liquid fluoride-salt cooled reactors. As part of the project, eight alloys were down-selected and fabricated in larger industrial scale heats by Haynes International. Resistance to molten salt was evaluated in flowing FLiNaK and FLiBe by Kairos Power using their Rotating Cage Loop (RCL) system. Accounting for iron deposition during these tests, the new alloys displayed very low net mass change showing excellent corrosion performance in molten salt. Creep properties evaluated at ORNL were found to be better than that of Hastelloy®N and 316 stainless steel. Long-term stabilities of the alloys evaluated by Haynes International showed that these alloys have excellent thermal stability in the temperature range 704.4-815.6°C, with the change in strength and ductility being less than 10-15% after a 4000-hour exposure at 815.6°C. Autogenously Gas Tungsten Arc Welding (GTAW) welded samples showed less than 10% change in yield strength / ultimate tensile strength / total elongation compared to the basemetal, indicating that the alloys have excellent weldability. Three parts were successfully investment-cast using one alloy with very little voiding showing feasibility of fabricating parts using the casting process. This project enabled extensive interaction between the material producer Haynes International, casting supplier MetalTek, and reactor developer Kairos Power. This facilitated testing of materials and components produced using the newly developed alloys by the end-user. This allowed the generation of critical dataset required for down-selection of a few promising alloys for further development. This data is also currently being shared with other reactor designers for them to evaluate the suitability of this alloy for their reactor design. The availability of this alloy will ultimately enable the design and development and deployment of MSRs with increased temperature of operation and thus, improved efficiencies.

36 MATERIALS SCIENCE↗