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At least 19 records

A FeCrAl-Al2O3 Composite Produced via Laser Powder Bed Fusion of a Mixed Powder for Porous Catalyst Scaffolds

This study proposes a novel approach for synthesizing and etching bicontinuous FeCrAl-Al2O3 composites as a means for replacing FeCrAl foams as catalyst scaffolds in bio-driven alcohol reactors for jet-fuel production. Conventional FeCrAl foams suffer from poor availability and consequent high costs. New additive manufacturing techniques provide an opportunity to produce tailored foams in reasonable times and at acceptable costs. This research aimed to generate a porous FeCrAl structure by etching a bicontinuous FeCrAl-Al2O3 composite produced by laser powder bed fusion of amalgamated FeCrAl and Al2O3 powders. The composite powder for laser powder bed fusion is created by ball-milling FeCrAl and Al2O3 powders. This research focuses on achieving a bi-continuous FeCrAl-Al2O3 structure, essential for the selective removal of the ceramic phase. The influence of laser processing parameters on the microstructure was examined across a range of laser powers (60-120 W) and scan speeds (100-400 mm/s), showing that higher powers and speeds produce finer metal struts. A bi-continuous microstructure was consistently obtained, marking a key achievement. The Al2O3 removal process involved a two-step etching method using hydrochloric and phosphoric acids, tested across various etching times. The alumina phase was reduced from 36 vol% to 17 vol% (corresponding to an increase in porosity from 24 vol% to 43 vol%), showing the potential for use as a porous catalyst scaffold. This research demonstrates the potential for using additive manufacturing to produce porous FeCrAl structures capable of replacing hard-to-source FeCrAl foams.

Son, Kwangtae

In situ self-ion (Fe + ) irradiation of ODS-FeCrAl alloy fuel cladding materials with different Cr contents: The early stages of Cr-rich α’ phase precipitation

Oxide-dispersion-strengthened FeCrAl (ODS-FeCrAl) alloys are candidate accident-tolerant fuel cladding materials for light water reactors because they demonstrate satisfactory resistance to materials degradation effects such as high-temperature oxidation, radiation-induced swelling, and creep. Their perspective deployment to market is challenged, however, by their inherent susceptibility to irradiation embrittlement caused by the precipitation of the brittle Cr-rich α’ phase at relatively low temperatures (≤475 °C). This work used in situ self-ion irradiation (150 keV Fe + ) in a transmission electron microscope to elucidate the early stages of Cr-rich α’ phase precipitation in three candidate ODS-FeCrAl alloy fuel cladding materials with different Cr contents (10, 12, and 20 wt.%) and microstructures. The early stages of the process resulting in the precipitation of the Cr-rich α’ phase in these three ODS-FeCrAl alloys under Fe + irradiation were investigated at room temperature and 300 °C up to total fluences of 1.7 × 10 15 ions·cm -2 (2 dpa) and 3.4 × 10 15 ions·cm -2 (4 dpa), using three damage dose rates (5 × 10 –5 , 3.3 × 10 –4 , and 2 × 10 –3 dpa·s -1 ). Post-irradiation examination via scanning transmission electron microscopy, energy-dispersive X-ray spectroscopy and electron energy loss spectroscopy suggested that the precipitation of the Cr-rich α’ phase might be promoted by the phase separation of the alloy matrix into Cr-rich and Fe-rich regions. Interestingly, oxygen impurities segregated preferentially in the Cr-rich regions, possibly promoting the radiation-assisted formation of the Cr-rich α’ phase. α’ phase precipitation was more pronounced at room temperature when compared to 300 °C, and it was clearly promoted by the progressive increase in the Cr content of the ODS-FeCrAl alloy.

36 MATERIALS SCIENCE

High‐Temperature Mechanical Behavior of Single‐Crystal FeCrAl Alloy Under In Situ Micropillar Compression

FeCrAl cladding is one of the candidate materials for the near‐term accident‐tolerant fuel technologies under development. Research on high‐temperature mechanical behaviors of single‐crystal FeCrAl alloy is rather limited. Previous studies have reported the mechanical property of low‐index orientation in single‐crystal FeCrAl alloy at room temperature. However, the critical resolved shear stress to activate slip systems can be orientation and temperature dependent. Here, single‐crystal grains in a coarse‐grained FeCrAl alloy with different crystallographic orientations are selected to preferentially activate {110}<111> slip systems or {112}<111> slip systems. Micropillars are fabricated in the selected single‐crystal grains and tested at elevated temperatures in situ in a scanning electron microscope. The critical resolved shear stresses of {110}<111> slip systems and {112}<111> slip systems are determined at various temperatures. The critical resolved shear stress shows a temperature dependence and orientation independence. This study provides important insight for understanding the deformation mechanisms of FeCrAl alloys at elevated temperatures.

Sun, Tianyi

Hydrogen permeation in iron-chromium-aluminum (FeCrAl) alloys and the effects of microstructure and surface oxide

Iron–chromium–aluminum (FeCrAl) class alloys are candidates for use as cladding for accident-tolerant fuels and moderators. In this context, hydrogen isotope permeation in FeCrAl alloys is an important material property. Here, in the present work, the apparent permeability, effective diffusivity, and apparent solubility of hydrogen in the FeCrAl alloys C26M and Kanthal D (KD) were measured with gas-driven hydrogen permeation. Permeation measurements were conducted at temperatures of 400 to 700 °C and at gas-driven pressures from 1 to 100 kPa. In particular, the effect of grain size on hydrogen transport was studied with KD samples with three different microstructures: nanocrystalline (NC), ultra-fine grained (UFG), and coarse-grained (CG). The UFG and NC specimens had higher apparent activation energies (73.4 kJ mol -1 and 65.2 kJ mol -1 , respectively) for hydrogen permeability than the CG sample (46.9 kJ mol -1 ). An aluminum oxide layer formed on the primary- and secondary-side surfaces of all samples subjected to permeation experiments which demonstrated the propensity of FeCrAl alloys to form these innate oxide permeation barriers.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

New insights on the effects of chemistry and temperature on α’ precipitation during aging of FeCrAl alloys

Here, the effect of Al on α' precipitation in FeCrAl alloys was studied through thermal aging of several model binary FeCr and FeCrAl alloys with Cr content of 13 wt.%, 17 wt.%, and 25 wt.% with and without 5.5 wt.% Al. Aging was performed up to 1,000h at varying temperatures from 400-500°C. At 400°C no age hardening was observed due to slow kinetics at this temperature. For both the 17Cr and 25Cr alloys, the addition of Al shows a lowering of the miscibility gap, consistent with other reports in literature. Interestingly, however, for the 25Cr alloys the addition of Al in the FeCrAl ternary alloy accelerated α' precipitation below the miscibility gap. Such enhanced precipitation has also been predicted by our atomistic kinetic Monte Carlo (AKMC) simulations. While previous literature has often focused on Al suppressing α', here we show that while Al can lower the miscibility gap in the Fe-Cr ferritic system thermodynamically, it may also enhance the kinetics of precipitation.

36 MATERIALS SCIENCE

A comparison of wrought and powder metallurgical FeCrAl claddings under simulated LWR accident transients

Iron-chromium-aluminum (FeCrAl) alloys are potential accident tolerant fuel (ATF) cladding candidates for light-water reactors but are difficult to fabricate as thin-walled tubes via conventional cast-and-wrought routes. Powder metallurgy (PM) offers a manufacturing alternative with improved compositional control, but its transient accident performance has not been directly benchmarked against wrought variants. This study evaluates the burst behavior of commercially developed PM-processed FeCrAl alloys, PM-C26M (Fe-12Cr-6Al-2Mo) and the high precipitate density FA-SMT (Fe-22Cr-5Al-3Mo), under simulated light-water reactor accident transient conditions. Burst testing was conducted using the Severe Accident Test Station with heating rates of 5 °C/s and 50 °C/s and internal pressures ranging from 25 MPa to 100 MPa. PM-C26M reproduced wrought C26M burst behavior within 7–37 °C across the stress range, indicating that PM processing does not compromise transient strength. FA-SMT exhibited markedly higher burst temperatures and reduced heating-rate sensitivity, consistent with its engineered precipitate strengthening. FA-SMT rupture exhibited axial "unzipping" rather than the lateral tearing characteristic of PM- and wrought C26M. Post-test EBSD and fractography indicate that this behavior is strongly correlated with strain-gated intergranular void nucleation associated with the dense precipitate architecture of FA-SMT, a response absent in the comparatively clean PM-C26M matrix and consistent with rupture morphologies reported for oxide-dispersion strengthened (ODS) FeCrAl of similar base-matrix chemistry to PM-C26M. These findings highlight the potential of powder metallurgy as a viable fabrication route for ATF claddings from an accident performance standpoint.

Bell, Sam [ORNL] (ORCID:0000000251905657)

Solid State Additive Manufacturing of Oxide Dispersion Strengthened-FeCrAl Alloy Components for High-Temperature Supercritical CO2 Power Cycle Applications

In this research, material extrusion additive manufacturing (MEAM) has been explored as an SSAM method for fabrication of 3-D components using ODS-FeCrAl alloy. MEAM-printed 3-D parts go through a series of process steps, e.g., chemical treatment, thermal treatment etc. in order to create a high density fully metallic part. Final 3-D part quality is associated with various process steps, e.g., filament fabrication, print design, and thermal treatment optimization. In MEAM, a metal powder loaded filament is used for printing 3-D shapes. Composition of the filament is very important since it provides shape retention at low-to-medium temperature. There are a few commercially available metallic alloy filaments. However, FeCrAl alloy filaments are not commercially available. In this project, we came up with a method to fabricate high quality composite FeCrAl filaments that could be used for MEAM printing. Subsequently, we have optimized MEAM print methods to fabricate samples that are larger than 10 mm, by using a modular print design approach. Finally, we have been able to optimize the chemical and high temperature heat treatment steps to achieve very high density (>98%) in sintered MEAM-printed products.

36 MATERIALS SCIENCE

Wrought FeCrAl alloy (C26M) cladding behavior and burst under simulated loss-of-coolant accident conditions

Cladding burst experiments for FeCrAl cladding were performed in the Severe Accident Test Station facility at Oak Ridge National Laboratory. These experiments were simulated using the BISON fuel performance code to better understand the cladding plastic behavior and failure under simulated loss-of-coolant accident conditions. 3D cladding surface boundary conditions were generated using composite axial and azimuthal profiles from experiment thermocouple data. To improve the simulation analysis capabilities in BISON for cladding burst behavior, new thermal creep, plasticity, and failure stress models specific to C26M, a wrought FeCrAl alloy, were developed and implemented. Initial cladding burst results indicated a general underprediction in the failure temperature of the six cladding burst simulations versus the observed failure temperatures. Close investigation of the experiment timing versus the underlying tensile test data revealed that, compared with the tensile specimens, the cladding tubes did not experience the same long holding time at high temperatures. New tensile tests were performed at high temperatures using a temperature ramp similar to the simulated loss-of-coolant accident experiments. These new tensile curves showed an approximately 80% increase in the ultimate tensile strength of the C26M alloy, indicating that a holding time of 10 min at 700 °C and 800 °C allows annealing to change the material microstructure. Using the updated tensile properties, the burst temperatures and stresses from the simulations showed remarkable agreement with the experimental results. This study was then extended by varying the initial pressure to highlight the burst temperature difference between standard Zircaloy-4 and C26M cladding under equivalent conditions. The results show that C26M has a burst temperature that is approximately 70–130 K greater than that of Zircaloy-4. In conclusion, these modeling predictions can be further improved by collecting high-temperature tensile data for C26M beyond the temperature ranges used in this work.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Radiation Damage Mitigation in FeCrAl Alloy at Sub-Recrystallization Temperatures

Traditional defect recovery methods rely on high-temperature annealing, often exceeding 750 °C for FeCrAl. In this study, we introduce electron wind force (EWF)-assisted annealing as an alternative approach to mitigate irradiation-induced defects at significantly lower temperatures. FeCrAl samples irradiated with 5 MeV Zr 2+ ions at a dose of 10 14 cm −2 were annealed using EWF at 250 °C for 60 s. We demonstrate a remarkable transformation in the irradiated microstructure, where significant increases in kernel average misorientation (KAM) and low-angle grain boundaries (LAGBs) typically indicate heightened defect density; the use of EWF annealing reversed these effects. X-ray diffraction (XRD) confirmed these findings, showing substantial reductions in full width at half maximum (FWHM) values and a realignment of peak positions toward their original states, indicative of stress and defect recovery. To compare the effectiveness of EWF, we also conducted traditional thermal annealing at 250 °C for 7 h, which proved less effective in defect recovery as evidenced by less pronounced improvements in XRD FWHM values.

FeCrAl alloys

Recrystallization driven softening and heating rate dependencies of FeCrAl nuclear fuel cladding during accident transients

A refined understanding of FeCrAl cladding behavior during rapid transients is critical for its potential deployment in light-water reactors. Current assessments focus on transient burst testing metrics such as balloon geometry, burst temperature, and hoop stress, often used as proxies for simpler conventional tensile properties. However, directly correlating isothermal tensile and creep data with accident transient scenarios remains a challenge, although it is essential for high fidelity model development. Recent modeling based on tensile tests up to 800 °C, conducted with both immediate loading and a 10-minute soak, showed that immediate loading better predicts experimental burst temperatures, indicating a thermal softening effect. Building upon this observation, the current study connects transient performance, microstructural evolution, and high-temperature tensile properties by leveraging results from C26M claddings burst tests performed at heating rates of 1–50 °C/s and hoop stresses from 25 to 100 MPa. At 25 MPa, rupture temperatures varied by only 6 °C, but at 100 MPa, the difference reached 116 °C, with faster heating yielding higher burst temperatures. Microstructural analysis identified recrystallization as the primary cause of heating rate-dependent softening, eliminating prior cold-working. In-situ thermomechanical data linked ballooning onset to localized instabilities, similar to ultimate tensile strength behavior in conventional tensile tests. High heating rates correlated with immediate loading tensile data, while lower rates matched soaked data. Furthermore, by linking burst performance to microstructural evolution and tensile properties, this work provides a foundation for more accurate modeling of FeCrAl claddings and potentially other Fe-based materials under accident conditions.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Production of Creep-Resistant FeCrAl-ODS

Four ODS FeCrAl alloys with base alloy composition Fe-16Cr-4Al-2Mo-0.2Y (wt.%) were mechanically alloyed with minor additions of CeO 2 and Y 2 O 3 additions and were successfully extruded into rectangular-shaped bars. Two oxide compositions were explored, which were designated NC with oxide addition of 0.5CeO 2 plus 0.2Yin solution of the base alloy powder and PC with additions of 0.5CeO 2 and 0.7Y 2 O 3 to elevate the O level. The microstructure of both alloys revealed by SEM and EBSD to consist of very small grains with sizes of ~450-520 nm and weak texture components. Sub-size tensile specimens fabricated from both alloys were tensile tested from room temperature to 800ºC. The results for both alloys from room temperature to 400ºC showed very high strengths, but low ductilities, especially uniform strain. From 500ºC to 800ºC, the strengths decreased rapidly, and the ductilities increased significantly. The reason for the rapid decreases in tensile strengths above 500ºC for both alloys is not clear, but will require advanced characterization techniques including atom probe tomography, to determine the size and number density of the nano-size oxide particles, and TEM/EFTEM, for investigating the dispersion of nano-size oxide particles on grain boundaries to assess the Zener grain boundary pinning effect, which will hinder grain coarsening at high temperatures that may enhance the Hall Petch strengthening mechanism.

36 MATERIALS SCIENCE

Long-term high-velocity oxidation and hot corrosion testing of several NiCrAl and FeCrAl base oxide dispersion strengthened alloys

Several oxide dispersion strengthened (ODS) alloys have been tested for cyclic, long-term, high gas-velocity resistance to oxidation at 1100 C and hot corrosion at 900 C. Both nominally Ni-16Cr-4Al and Fe-20Cr-4.5Al ODS alloys were subjected up to about 2500 cycles, where each cycle consisted of 1 hr in a hot, Mach 0.3 combusted gas stream followed by a 3-min quench in an ambient temperature, Mach 0.3 air blast. For comparison to existing technology, a coated superalloy was simultaneously tested. The ODS iron alloy exhibited clearly superior behavior, surviving 3800 oxidation and 2300 hot corrosion cycles essentially unscathed. While the ODS nickel alloys exhibited adequate oxidation resistance, the long-term hot corrosion resistance could be marginal, since the best life for such alloys under these conditions was only about 1100 cycles. However, the hot corrosion resistance of the ODS Ni-base alloys is excellent in comparison to that of traditional superalloys.

Lowell, C. E.

Development and Evaluation of Embrittlement Resistant Alloys for Advanced LWR Cladding

The primary challenge preventing the deployment of reactor designs that leverage wrought FeCrAl as an advanced light-water reactor (LWR) cladding is irradiation hardening and embrittlement. Wrought FeCrAl alloys experience a loss of post-irradiation ductility and fracture toughness under low-temperature neutron irradiation (< 350°C) resulting from the combined effects of dislocation loop formation and the irradiation-enhanced precipitation of Cr-rich alpha-prime precipitates throughout the microstructure. Over the past decade, significant improvements in our understanding regarding the effect of Cr and Al content have been enabled through neutron irradiations, but even optimized wrought alloys such as C26M remain vulnerable to brittle failure during storage, transportation, and handling following irradiation. This report summarizes multiple irradiation campaigns initiated over the past 7 years and provides recent insights into the effect of (1) minor alloying composition, (2) alloy processing strategy, (3) crystal structure, and (4) the use of advanced oxide dispersion strengthened (ODS) alloys. The first irradiation campaign irradiated body-centered cubic FeCrAl alloy C26M with and without elements such as Mo and Y. It also included face-centered cubic alumina-forming austenitic (AFA) alloys that have a steeper neutronic penalty but that have far superior high-temperature strength than wrought FeCrAl. Finally, this campaign compared conventional wrought C26M with the same material produced using modern powder metallurgical hotisostatic pressing (PM-HIP). The second irradiation campaign, initiated in 2018, irradiated wrought and FeCrAl-ODS materials up to 50 dpa to assess their irradiation resistance to high-doses. The results of this work indicate that wrought C26M suffers significant degradation following neutron irradiation at LWR-relevant temperatures regardless of Mo and Y content. The PM-HIP variant appears to be more resilient to irradiation-induced ductility loss in comparison with wrought variants but still loses almost all ductility by 8 dpa. Notably, the AFAs retained at least 5% total elongation after irradiation at the same dose and temperature condition, although additional deterioration may be expected at higher fluence levels. FeCrAl-ODS materials show the greatest promise as a transformative longer-term accident-tolerant fuel (LT-ATF) cladding material. The extruded 106ZY10C alloy retained 10% total elongation after 16 dpa irradiation and retained 8% total elongation after 50 dpa. Additional challenges with FeCrAl-ODS alloys also remain, including optimization of end cap joining methodologies, enhancement of fracture toughness, scaling production to prove economic viability, and optimizing post-pilger heat treatments to maximize ductility and irradiation resistance. This series of irradiations demonstrates the efficacy of the LWR testbed available within the United States for the rapid irradiation and down-selection of LT-ATF candidates. As the country rapidly accelerates its timeline for the deployment of advanced reactor concepts, the effective utilization of the High Flux Isotope Reactor for separate-effects style irradiations should continue to be prioritized to answer the final questions pertaining to LT-ATF candidates necessary for the deployment of advanced boiling water reactors and small modular reactors.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Bonding of vanadium- and Iron-based alloys as interlayers for plasma-facing and structural materials in fusion systems

Vanadium alloys and FeCrAl were investigated as interlayers between tungsten and reduced activation ferritic martensitic steel for fusion system components to avoid formation of intermetallic phase at operating temperatures between 550 and 1100 °C, while maintaining a body centered cubic phase throughout the interface. Physical and mechanical properties need to be graded between tungsten and steel, but recent results showed a significant hardness increase at the FeCrAl to vanadium alloy interface. Here, a sintered sample of these alloys was annealed for extended time, and the microstructure was investigated to provide a better understanding of the phenomena. A comparison with an additively manufactured interface of the same material is provided. An unexpected L2 1 intermetallic phase formation has been revealed using microscopy and synchrotron techniques and will inform future additive manufacturing approaches of the interface. A Cr layer interface as a preliminary solution was proposed between the Vanadium alloy and FeCrAl alloy interface.

Additive manufacturing

Embedded Aluminum Nitride Sensors for Advanced Reactors

This project aims to manipulate the of growth of aluminum nitride (AlN) inclusions in an iron-chromium-aluminum (FeCrAl) alloy, using the principle of powder metallurgy and heat treatment methods. to promote the formation of AlN phase within FeCrAl for embedded sensing. This effort seeks to fill in a gap with respect to robust sensor hardware for ubiquitous structural health monitoring of advanced nuclear reactors. A systematic evaluation of various solid-state methods will be performed to understand the influence of process conditions on AlN growth and to promote the growth of desirable AlN phase. Fabricated specimens will be analyzed to investigate the AlN structures that are formed using a suite of tools to characterize the concentration, morphology, and distribution of AlN within the FeCrAl substrate.

22 GENERAL STUDIES OF NUCLEAR REACTORS

Diffusivity in Alumina Scales Grown on Al-MAX Phases

Ti3AlC2, Ti2AlC, and Cr2AlC are oxidation resistant MAX phase compounds distinguished by the formation of protective Al2O3 scales with well controlled kinetics. A modified Wagner treatment was used to obtain interfacial grain boundary diffusivity, deltaD(sub gb,O,int.), from scale growth rates and corresponding grain size. It is based on the p(O2)(exp -1/6) dependency of the double charged oxygen vacancy and oxygen diffusivity, coupled with the effective diffusion constant for short circuit grain boundary paths. Data from the literature for MAX phases was analyzed accordingly, and deltaD(sub gb,O,int.) was found to nearly coincide with the Arrhenius line developed for Zr-doped FeCrAl, where: deltaD(sub gb,O,int.) = 1.8x10(exp -10) exp(-375 kJ/RT) cubic meters/s. Furthermore, this oxidation relation suggests the more general format applicable to bulk samples under ambient conditions: deltaD(sub gb,O) = 7.567x10(exp -8) exp(-544 kJ/RT) p(O2)(exp -1/6) cubic meters/[s x Pa(exp -1/6)]. Data from many other FeCrAl(X) studies were similarly assessed to show general agreement with the relation for deltaD(sub gb,O,int.). This analysis reinforces the view that protective alumina scales grow by similar mechanisms for these Al-MAX phases and oxidation resistant FeCrAl alloys.

aluminum oxide