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Tritium embrittlement of austenitic stainless-steel tubing at low helium contents
Austenitic stainless steels are the standard materials for containment of hydrogen and tritium because of their resistance to mechanical property degradation in those environments. The mechanical performance of the primary containment material is critical for tritium handling, processing, and storage, thus comprehensive understanding of the processes of tritium embrittlement is an enabling capability for fusion energy. This work describes the investigation of the effects of low levels of tritium-decay-helium ingrowth on 304 L tubes. Long-term aging with tritium leads to high helium contents in austenitic stainless steels and can reduce fracture toughness by 95 %, but the details of behavior at low helium contents are not as well characterized. Here, we present results from tensile testing of tritium pre-charged 304 L tube specimens with a variety of starting microstructures that all contain a low level of helium. The results of the tritium exposed-and-aged materials are compared to previously reported results on similar specimens tested in an unexposed condition as well as the hydrogen precharged condition. Tritium precharging and aging for a short duration resulted in increased yield strengths, ultimate tensile strengths and slightly increased elongation to failure, comparable to higher concentrations of hydrogen precharging.
Friction Stir Dovetailing of AA7099 to Steel with AA6061 Interlayer for Reduced Zn Embrittlement at Dissimilar Interface
Joining of high strength Al alloy (AA7099) to steel (rolled homogeneous armor) with and without AA6061 interlayer was achieved using a friction stir dovetailing (FSD) method. Detailed investigations were conducted to establish correlations between mechanical performance and microstructural evolution of FSD joints. Lap shear tensile testing revealed that incorporation of the AA6061 interlayer combined with tailored processing methodology significantly improved both mechanical interlocking and load transmission across the dovetail interface. Following incorporation of the interlayer, the maximum load carrying capacity and peak extension (of the AA7099/AA6061/steel joint) are 60% and 210% higher, respectively, than results obtained from an AA7099/steel joint without an interlayer. Without an AA6061 interlayer, formation of zinc rich intermetallic compounds led to brittle interfacial failure of the AA7099-steel FSD joint. Incorporation of novel tool and joint configuration eliminated asymmetric joint performance as a function of loading direction, which is generally observed in friction stir lap welding. The efficacy of the use of an AA6061 interlayer in joining AA7099 to steel was demonstrated through mechanical testing as well as high resolution analytical electron microscopy characterization.
Spectrum of embrittling potencies and relation to properties of symmetric-tilt grain boundaries
Grain boundaries in metallic materials can exist in a wide range of stable and metastable structures. In addition, the properties of a grain boundary may be altered through solute segregation. In this work, we present a formulation that combines the spectrum of embrittling potencies associated with solute segregation with site-occupancy statistics. As a prototype problem, we illustrate the relation between segregation and embrittlement in the case of S segregation to grain boundaries in Ni. To obtain a population of site segregation energies, we perform molecular statics calculations on 378 different symmetric-tilt grain boundaries and their free surface equivalents, using an embedded-atom method interatomic potential developed specifically for studying embrittlement. Our results show that it is important to consider both the energies associated with embrittlement and the probability of occupancy to describe the general embrittling nature of a grain boundary. When analyzed in isolation, certain grain boundaries show large embrittling potencies; however, that effect is diminished when the probability of S segregation to that grain boundary is considered within a polycrystal. We propose a new quantity, the embrittling estimator, which not only categorizes grain boundaries as embrittling or strengthening, but also considers site occupancy probabilities, so that the embrittlement behavior of grain boundaries within a network of grain boundaries can be compared. Finally, we examine the relationship between embrittlement behavior and innate grain boundary properties, such as the free volume, and find statistical evidence that the complex nature of embrittlement cannot be explained by linear correlations with excess volumes or energies. Ultimately, this combined approach provides a theoretical tool to assist grain boundary engineering of metastable alloys.
Statistical perspective on embrittling potency for intergranular fracture
Embrittling potency is a thermodynamic metric that assesses the influence of solute segregation to a grain boundary (GB) on intergranular fracture. Historically, authors of studies have reported embrittling potency as a single scalar value, assuming a single segregation site of importance at a GB and a particular cleavage plane. However, the topography of intergranular fracture surfaces is not generally known a priori. Accordingly, we, in this study, present a statistical ensemble approach to compute embrittling potency, where many free surface (FS) permutations are systematically considered to model fracture of a GB. The result is a statistical description of the thermodynamics of GB embrittlement. As a specific example, embrittling potency distributions are presented for Cr segregation to sites at two Ni $\langle 111 \rangle$ symmetric tilt GBs using atomistic simulations. We show that the average embrittling potency for a particular GB site, considering an ensemble of FS permutations, is not equal to the embrittling potency computed using the lowest energy pair of FSs. A mean GB embrittlement is proposed, considering both the likelihood of formation of a particular FS and the probability of solute occupancy at each GB site, to compare the relative embrittling behavior of two distinct GBs.
The Effect of Grain Boundary Facet Junctions on Segregation and Embrittlement
Junctions are discontinuities in flat grain boundaries that arise in all polycrystalline materials and are thought to play important roles in the response of a grain boundary network to thermal and mechanical loads. A key open question concerns the mechanisms by which solute segregation to junctions impacts properties of the grain boundary. Here, in this work, we investigate the influence of grain boundary facet junctions on solute embrittlement, and we present an analytical model that uses the hydrostatic stress field contributed by dislocations at multiple junctions to describe these effects. Specifically, we study junctions between {112} facets of various lengths in Au $\langle111\rangle$ Σ3 tilt grain boundaries. Copper and silver solutes are employed to determine if the effect of junctions on solute segregation and embrittlement is dependent on size relative to the host. Combined, atomistic simulation data and the analytical model show that Cu and Ag have opposite segregation responses to junctions due to the sign of the hydrostatic stress field induced by junctions. However, a positive shift in the embrittling potency is computed near junctions regardless of solute type or the stress state of the segregation site. Hence, for the conditions studied, junctions consistently shift the energetic landscape towards embrittlement.
Assessment of irradiation embrittlement effect on fatigue life of a pressurized-water reactor pressure vessel using the fracture toughness master curve approach
The reactor pressure vessel (RPV) is a critical structural component in pressurized-water reactors, and it is designed to withstand extreme conditions, such as high pressures, elevated temperatures, and prolonged radiation exposure. Ensuring RPV integrity is essential for the safe and reliable long-term operation of nuclear power plants, especially as aging mechanisms such as fatigue and irradiation embrittlement pose increased risks. Fatigue, caused by cyclic thermal and mechanical loading, can lead to crack initiation in localized high-stress regions. Simultaneously, neutron irradiation, particularly in the beltline region, progressively reduces fracture toughness, increasing susceptibility to brittle fracture. These combined effects of fatigue and irradiation embrittlement potentially impact the RPV structural integrity, necessitating fitness-for-service assessments. This study applies the fracture toughness master curve approach to evaluate the impact of irradiation embrittlement on RPV fatigue life. A coupled thermo-mechanical stress analysis identifies critical stress locations under normal service transients, pinpointing regions most vulnerable to fatigue crack initiation and growth. Stress intensity factors for postulated flaws at these locations are calculated, enabling an assessment of fatigue life under irradiated and unirradiated conditions. The results indicate that neutron irradiation embrittlement accelerates the conditions in which a critical crack can form and lead to failure, particularly at lower temperatures. The failure occurs where reduced fracture toughness limits the material’s resistance to crack growth. Axial cracks at nozzle corners are the most life limiting without irradiation, while circumferential cracks demonstrate longer fatigue lives. The findings highlight the importance of incorporating irradiation effects into fatigue life predictions to ensure the long-term structural integrity of RPVs.
On High-Fluence Irradiation Hardening of Nine RPV Surveillance Steels in the UCSB ATR-2 Experiment: Implications for Extended-Life Embrittlement Predictions
Nine archival reactor pressure vessel (RPV) surveillance steels from commercial nuclear power plants were irradiated in the University of California, Santa Barbara Advanced Test Reactor 2 (ATR-2) experiment to evaluate irradiation embrittlement under low-flux surveillance capsule versus higher flux test reactor (ATR-2) conditions. The postirradiation measurements of irradiation hardening, measured as increases in yield stress (Δσy), and corresponding conversions of Δσy to Charpy V-notch 41-J transition temperature shifts (ΔTc) are compared with various embrittlement trend curve (ETC) model predictions for the nine steels. Tensile and converted shear punch and microhardness measurements of Δσy generally show a continuing increase between intermediate and high ATR-2 fluences. The Eason-Odette-Nanstad-Yamamoto and ASTM E900 ETC models underpredict embrittlement at the ATR-2 irradiation condition: irradiation temperature (Ti) of 292°C, neutron fluence (ϕt) of 1.4 × 1020 n/cm2 (E > 1 MeV), and neutron flux (ϕ) of 3.68 × 1012 n/cm2-s. On average, the French FIS and Japanese JAEC ETCs slightly overpredict the ATR-2 data. The increase in Δσy with higher fluence is primarily due to Ni-Mn-Si precipitates, which slowly evolve in both nearly copper-free and copper-bearing steels. Finally, a new Odette-Wells-Almirall-Yamamoto embrittlement model is shown that yields good predictions for the nine steels at high fluences (ϕt > 5.5 × 1019 n/cm2).
On High-Fluence Irradiation Hardening of Nine RPV Surveillance Steels in the UCSB ATR-2 Experiment: Implications for Extended-Life Embrittlement Predictions
Nine archival reactor pressure vessel (RPV) surveillance steels from commercial nuclear power plants were irradiated in the University of California, Santa Barbara Advanced Test Reactor 2 (ATR-2) experiment to evaluate irradiation embrittlement under low-flux surveillance capsule versus higher flux test reactor (ATR-2) conditions. The postirradiation measurements of irradiation hardening, measured as increases in yield stress (Δσy), and corresponding conversions of Δσy to Charpy V-notch 41-J transition temperature shifts (ΔTc) are compared with various embrittlement trend curve (ETC) model predictions for the nine steels. Tensile and converted shear punch and microhardness measurements of Δσy generally show a continuing increase between intermediate and high ATR-2 fluences. The Eason-Odette-Nanstad-Yamamoto and ASTM E900 ETC models underpredict embrittlement at the ATR-2 irradiation condition: irradiation temperature (Ti) of 292°C, neutron fluence (ϕt) of 1.4 × 1020 n/cm2 (E > 1 MeV), and neutron flux (ϕ) of 3.68 × 1012 n/cm2-s. On average, the French FIS and Japanese JAEC ETCs slightly overpredict the ATR-2 data. The increase in Δσy with higher fluence is primarily due to Ni-Mn-Si precipitates, which slowly evolve in both nearly copper-free and copper-bearing steels. Finally, a new Odette-Wells-Almirall-Yamamoto embrittlement model is shown that yields good predictions for the nine steels at high fluences (ϕt > 5.5 × 1019 n/cm2).
Characterizing the flux effect on the irradiation embrittlement of reactor pressure vessel steels using machine learning
In-service exposure to high-energy neutrons embrittles reactor pressure vessel (RPV) steels. An increase in the yield stress (Δσ y ) results in a corresponding increase in the brittle to ductile transition temperature (ΔT c ). Most existing models underpredict ΔT c at higher fluence following accelerated irradiations in test reactors. High fluence, up to 10 20 n/cm 2 in some cases, will be reached over extended RPV vessel operation of 80 years, or more, at low service flux. Embrittlement has been extensively studied in accelerated, higher flux test reaction irradiations. However, the use of test reactor data naturally raises the question of flux effects. Here, this study used a machine learning approach trained on a set of hardening data, covering a wide range of flux, fluence, and steel compositions to determine the interactive effects of both irradiation and material variables on Δσ y . The analysis included machine learning-based cross-plots of the variable dependence of Δσ y for six core steels (i.e., CM6, LC, LD, LG, LH, and LI), with controlled differences in their Cu and Ni contents. A primary objective is to evaluate an effective to actual fluence (Φt e /Φt) ratio, as a function of flux, fluence, and steel composition. This is information critical to properly use intermediate flux-high fluence data in calibrating a low flux-high fluence embrittlement model. The predicted Φt e /Φt is reasonably consistent with estimates previously derived from a physics-based solute recombination trap model.
Detection of voids in hydrogen embrittled iron using transmission X-ray microscopy
Hydrogen embrittlement remains a barrier to widespread adoption of hydrogen as a carbon-neutral energy source. Here, hydrogen embrittlement mechanisms are investigated across length scales in iron using transmission X-ray microscopy (TXM), digital image correlation (DIC), and notched tensile testing during in-situ electrochemical hydrogen charging. TXM reveals void size and spatial distribution ahead of a propagating crack. We find hydrogen charging leads to voids within ~10 μm of the crack tip and suppression of voids beyond this distance. Near the crack tip, voids are elongated in the direction of the crack and are smaller than voids in an uncharged sample. In the presence of hydrogen, these voids lead to quasi-cleavage fracture and a sharper crack tip. DIC shows localization and reduction of plastic strain with hydrogen charging, and tensile testing reveals a reduction in fracture energy and elongation at failure. Finally, these results are discussed in the context of hydrogen embrittlement mechanisms.
Hydrogen Embrittlement of Medium Mn Steels
Recent research efforts to develop advanced–/ultrahigh–strength medium-Mn steels have led to the development of a variety of alloying concepts, thermo-mechanical processing routes, and microstructural variants for these steel grades. However, certain grades of advanced–/ultrahigh–strength steels (A/UHSS) are known to be highly susceptible to hydrogen embrittlement, due to their high strength levels. Hydrogen embrittlement characteristics of medium–Mn steels are less understood compared to other classes of A/UHSS, such as high Mn twinning–induced plasticity steel, because of the relatively short history of the development of this steel class and the complex nature of multiphase, fine-grained microstructures that are present in medium–Mn steels. The motivation of this paper is to review the current understanding of the hydrogen embrittlement characteristics of medium or intermediate Mn (4 to 15 wt pct) multiphase steels and to address various alloying and processing strategies that are available to enhance the hydrogen-resistance of these steel grades.
Use of Mini-CT Specimens for Fracture Toughness Characterization of Irradiated Highly Embrittled Weld
In the 1990’s, the Heavy Section Steel Irradiation Program at the ORNL performed investigation of the shape of the fracture toughness master curve for reactor pressure vessel steel highly embrittled because of irradiation exposure. A radiation-sensitive reactor pressure vessel (RPV) weld with intentionally enhanced copper content, designated KS-01, has been characterized in terms of static initiation (KJc) and Charpy impact toughness in the unirradiated and irradiated conditions. The objective of this original project was to investigate the ability of highly embrittled material to maintain the shape of the unirradiated transition fracture toughness curve, as well as to examine the ability of the Charpy 41-J shift to predict the fracture toughness shift at such high level of embrittlement. Irradiation of this weld was performed at the University of Michigan Ford Reactor in the new HSSI irradiation-anneal-reirradiation (IAR) facility. Broken specimens from that project have been saved in ORNL storage. To verify applicability of Mini-CT specimens for fracture toughness characterization of RPV materials as part of the DOE Light Water Reactor Sustainability Program, Mini-CT specimens were machined from broken Charpy specimens and tested according to ASTM E1921 standard. As result of this study, the fracture toughness of this weld derived by testing Mini-CT specimens in the unirradiated and irradiated conditions is compared to previously reported fracture toughness derived by large number of conventional specimens.
Impact of Gold Thickness on Interfacial Evolution and Subsequent Embrittlement of Tin–Lead Solder Joints
Although gold remains a preferred surface finish for components used in high-reliability electronics, rapid developments in this area have left a gap in the fundamental understanding of solder joint gold (Au) embrittlement. Furthermore, as electronic designs scale down in size, the effect of Au content is not well understood on increasingly smaller solder interconnections. As a result, previous findings may have limited applicability. The current study focused on addressing these gaps by investigating the interfacial microstructure that evolves in 63Sn-37Pb solder joints as a function of Au layer thickness. Those findings were correlated to the mechanical performance of the solder joints. Increasing the initial Au concentration decreased the mechanical strength of a joint, but only to a limited degree. Kirkendall voids were the primary contributor to low-strength joints, while brittle fracture within the intermetallic compounds (IMC) layers is less of a factor. The Au embrittlement mechanism appears to be self-limiting, but only once mechanical integrity is degraded. Sufficient void evolution prevents continued diffusion from the remaining Au.
Evaluation of liquid metal embrittlement of F82H and 4340 steels in liquid lithium
Here, to evaluate the liquid metal embrittlement (LME) susceptibility of F82H, a reduced activation ferritic-martensitic (RAFM) steel, a testing procedure using hollow cylindrical tensile specimens was used. Tensile tests are compared between specimens filled with argon and lithium at 200 °C. To validate the procedure, initial testing was performed on type 4340 steel, which is well-known to exhibit LME. Compared to 4340 steel, F82H only showed minor effects of Li exposure, including pre-testing exposures with Li at 400 °C for 1 h and 500 °C for 500 h. Furthermore, changing the strain rate or tensile test temperature also did not show significant embrittlement.
Hydrogen embrittlement and mechanical response of 304L steel with ZrC additions
While stainless steels are widely used for hydrogen storage infrastructure, they can still be vulnerable to hydrogen embrittlement justifying the need to further improve their hydrogen resiliency. Here, we investigate the potential for transition metal carbide additions to improve the hydrogen compatibility of austenitic stainless steels. ZrC nanoparticles were dispersed in contents of 0.01–10 wt% in 304 L stainless steel powder, mixed via high energy ball milling, and subsequently consolidated using direct current sintering. To assess hydrogen compatibility, the tensile properties of similarly processed 304 L without ZrC nanoparticles were compared to 304 L with the ZrC additions; both materials were evaluated prior to and after hydrogen exposure (non-charged and H-precharged, respectively). Depending upon the ZrC phase fraction, the yield strengths varied from ∼325 to 560 MPa in the non-charged condition and from ∼375 to 550 MPa in the H-precharged condition. Strain at failure varied from ∼5 to 90 % and from ∼5 to 35 % in the non-charged and hydrogen-precharged conditions, respectively. Results from stress-strain profiles demonstrate limited efficacy of ZrC as a method to mitigate hydrogen embrittlement entirely but does demonstrate the potency of ZrC inclusions as strengthening addition to 304 L alloys without a loss of ductility.
Fast Neutron Irradiation Embrittlement-ductilitization of an Iron-based Amorphous Alloy using In Situ Synchrotron X-ray Diffraction
Amorphous Fe-based nanostructured alloy coatings thermally sprayed on bcc steel substrate, were subjected to neutron irradiation doses up to 2 × 10 19 n/cm 2 . It is shown that the interplay between embrittlement and recovery of ductility is governed by amorphous to crystallization transition and phase decomposition in which temperature and irradiation dose have reciprocal effects. Microscopic (X-ray diffraction) observations on the behavior of the amorphous Fe-based alloy are correlated with relevant macroscopically observed mechanical behavior. It is shown that amorphous Fe-based alloy coatings maintain and even enhance their amorphous structure with irradiation, exhibit radiation-induced restoration of thermally-induced embrittlement and finally exhibit resistance to ductility loss up to the fluence of 2 × 10 18 n/cm 2 and good thermal stability up to 350 °C. The latter is deduced from X-ray diffraction experiments of in-situ tensile strain application on the irradiated coating.
Electrochemical pumping: An alternative solution for hydrogen embrittlement
Hydrogen embrittlement is a form of chemo-mechanical damage that is special in that it can be partially reversible. Here, in this paper, we propose a method for recovering structural alloys from hydrogen embrittlement at room temperature by electrochemically biased desorption of hydrogen. We demonstrate that the method can enable the reversion of hydrogen-induced degradation of mechanical properties, by comparing the mechanical behavior of commercial stainless steel specimens at different hydrogen charging and desorption states. These case studies also reveal the influence of electrochemical potential, H content and the characteristics of H trapping sites, on the effectiveness of this recovery approach. The limitations arising from the presence of unhealable forms of hydrogen damage, and the generic applicability of this electrochemically-assisted recovery method are also discussed.