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DOE OSTI2023

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).

Nanstad, Randy K.↗

NASA NTRS1972

Environmental hydrogen embrittlement of an alpha-beta titanium alloy - Effect of microstructure.

Study of environmental hydrogen embrittlement of a Ti-6 Al-4 alloy as a function of test displacement rate and of variations in alpha-beta microstructure. Embrittlement in low-pressure (about 1 atm) gaseous hydrogen was inversely dependent on test displacement rate and strongly dependent on microstructure. At a given displacement rate, microstructures having a continuous alpha-phase matrix were less severely embrittled than those having a continuous beta-phase matrix. Further, brittle fracture occurred in the former microstructures by transgranular cleavage and in the latter microstructures by intergranular separation. These observations are consistent with previous studies made on slow strain-rate embrittlement of hydrogen-charged titanium alloys and are explained in terms of relative hydrogen transport rates within the alpha-phase and beta-phase titanium.

Nelson, H. G.↗

NASA NTRS1975

Effects of alloy composition in alleviating embrittlement problems associated with the tantalum alloy T-111

The causes of aging embrittlement in T-111 (Ta-8W-2Hf) and the effect of alloy modification were investigated. Results show that T-111 possesses a critical combination of tungsten and hafnium that leads to loss in ductility at -196 C after aging near 1040 C. It was found that this occurs because tungsten enhances hafnium segregation to grain boundaries, which also leads to increased susceptibility to hydrogen embrittlement. Aging embrittlement was not observed in tantalum alloys with reduced tungsten or hafnium contents; most of the alloys studied have lower strengths than T-111 and exhibit susceptibility to hydrogen embrittlement.

Stephens, J. R.↗

NASA NTRS1977

Effects of alloy composition in alleviating embrittlement problems associated with the tantalum alloy T-111

The causes of aging embrittlement in T-111 (Ta-8W-2Hf) and the effects of alloy modification were investigated. Results showed that T-111 contains a critical combination of tungsten and hafnium that leads to loss of ductility at -196 C after aging near 1040 C. This appears to occur because tungsten enhances hafnium segregation to grain boundaries and this also leads to increased susceptibility to hydrogen embrittlement. Aging embrittlement was not observed in tantalum alloys with reduced tungsten or hafnium contents; however, most of the alloys studied have lower strengths than T-111 and exhibit susceptibility to hydrogen embrittlement.

Stephens, J. R.↗

NASA NTRS1996

Technique to Predict Ultraviolet Radiation Embrittlement of Polymers in Space

In the low-Earth-orbit environment, solar ultraviolet (UV) radiation embrittles polymer materials through bond breaking and crosslinking. This UV embrittlement increases the surface hardness of the polymer. Before the durability of polymer materials in the low- Earth-orbit environment can be predicted, the extent of UV embrittlement needs to be determined. However, traditional techniques for measuring the microhardness of materials cannot be employed to measure changes in the hardness of UV-embrittled surfaces because traditional techniques measure bulk hardness and are not sensitive enough to surface changes. A unique technique was used at the NASA Lewis Research Center to quantify polymer surface damage that had been induced by UV radiation. The technique uses an atomic force microscope (AFM) to measure surface microhardness. An atomic force microscope measures the repulsive forces between the atoms in a microscopic cantilevered tip and the atoms on the surface of a sample. Typically, an atomic force microscope produces a topographic image of a surface by monitoring the movement of the tip over features of the surface. The force applied to the cantilevered tip, and the indention of the tip into the surface, can be measured. The relationship between force and distance of indentation, the quantity force/distance (newtons/meter), provides a measure of the surface hardness. Under identical operating conditions, direct comparisons of surface hardness values can be made.

Source record↗

NASA NTRS2008

Nickel-Based Superalloy Resists Embrittlement by Hydrogen

A nickel-based superalloy that resists embrittlement by hydrogen more strongly than does nickel alloy 718 has been developed. Nickel alloy 718 is the most widely used superalloy. It has excellent strength and resistance to corrosion as well as acceptably high ductility, and is recognized as the best alloy for many high-temperature applications. However, nickel alloy 718 is susceptible to embrittlement by hydrogen and to delayed failure and reduced tensile properties in gaseous hydrogen. The greater resistance of the present nickel-based superalloy to adverse effects of hydrogen makes this alloy a superior alternative to nickel alloy 718 for applications that involve production, transfer, and storage of hydrogen, thereby potentially contributing to the commercial viability of hydrogen as a clean-burning fuel. The table shows the composition of the present improved nickel-based superalloy in comparison with that of nickel alloy 718. This composition was chosen to obtain high resistance to embrittlement by hydrogen while maintaining high strength and exceptional resistance to oxidation and corrosion. The most novel property of this alloy is that it resists embrittlement by hydrogen while retaining tensile strength greater than 175 kpsi (greater than 1.2 GPa). This alloy exhibits a tensile elongation of more than 20 percent in hydrogen at a pressure of 5 kpsi (approximately equal to 34 MPa) without loss of ductility. This amount of elongation corresponds to 50 percent more ductility than that exhibited by nickel alloy 718 under the same test conditions.

Lee, Jonathan↗

DOE OSTI2023

On High-Fluence Irradiation Hardening of Nine RPV Surveillance Steels in the UCSB ATR-2 Experiment: Implications for Extended-Life Embrittlement Predictions

Nanstad, Randy↗

DOE OSTI2023

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.

36 MATERIALS SCIENCE↗

DOE OSTI2022

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.

08 HYDROGEN↗

DOE OSTI2021

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.

36 MATERIALS SCIENCE↗

DOE OSTI2022

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.

Sokolov, Mikhail A.↗

NASA NTRS1973

Hydrogen environment embrittlement of metals

Hydrogen environment embrittlement refers to metals stressed while exposed to a hydrogen atmosphere. Tested in air, even after exposure to hydrogen under pressure, this effect is not observed on similar specimens. Much high purity hydrogen is prepared by evaporation of liquid hydrogen, and thus has low levels for potential impurities which could otherwise inhibit or poison the absorbent reactions that are involved. High strength steels and nickel-base allows are rated as showing extreme embrittlement; aluminum alloys and the austenitic stainless steels, as well as copper, have negligible susceptibility to this phenomenon. The cracking that occurs appears to be a surface phenomenon, is unlike that of internal hydrogen embrittlement.

Jewett, R. P.↗

NASA NTRS1973

Role of Hf and Zr in the hydrogen embrittlement of Ta and Cb alloys

The hydrogen embrittlement of aged T-111 and similar Ta and Cb alloys is characterized and the mechanisms believed responsible for the increased sensitivity of T-111 to low temperature hydrogen embrittlement after aging for 1000 hours or longer near 1040 C are described. A total of eight Ta base alloys and two Cb base alloys were investigated. The effects of pre-age annealing temperature, aging time, temperature and environment, and alloy composition on the susceptibility to hydrogen embrittlement were investigated. The primary method of determining the effects of these variables on the ductility of T-111 was by bend testing at 25 and -196 C. Fractured specimens were examined by the scanning electron microscope, electron microprobe, metallography and X-ray diffration.

Stephens, J. R.↗

NASA NTRS1973

Aqueous chloride stress corrosion cracking of titanium: A comparison with environmental hydrogen embrittlement

The physical characteristics of stress corrosion cracking of titanium in an aqueous chloride environment are compared with those of embrittlement of titanium by a gaseous hydrogen environment in an effort to help contribute to the understanding of the possible role of hydrogen in the complex stress corrosion cracking process. Based on previous studies, the two forms of embrittlement are shown to be similar at low hydrogen pressures (100 N/sqm) but dissimilar at higher hydrogen pressures. In an effort to quantify this comparison, tests were conducted in an aqueous chloride solution using the same material and test techniques as had previously been employed in a gaseous hydrogen environment. The results of these tests strongly support models based on hydrogen as the embrittling species in an aqueous chloride environment. Further, it is shown that if hydrogen is the causal species, the effective hydrogen fugacity at the surface of titanium exposed to an aqueous chloride environment is equivalent to a molecular hydrogen pressure of approximately 10 N/sqm.

Nelson, H. G.↗

NASA NTRS1974

Role of HF and Zr in the hydrogen embrittlement of Ta and Cb alloys

An attempt is made to characterize the hydrogen embrittlement of aged T-111 and similar Ta and Cb alloys and to describe the mechanisms believed responsible for the increased sensitivity of T-111 to low temperature hydrogen embrittlement after aging for 1000 hr or longer near 1040 C. A total of eight Ta-base alloys and two Cb-base alloys were investigated. The effects of pre-age annealing temperature, aging time, temperature and environment, and alloy composition on the susceptibility to hydrogen embrittlement were investigated. The primary method of determining the effects of these variables on the ductility of T-111 was by bend testing at 25 and -196 C. Fractured specimens were examined by the scanning electron microscope, electron microprobe, metallography, and X-ray diffraction.

Stephens, J. R.↗

NASA NTRS1974

Aqueous chloride stress corrosion cracking of titanium - A comparison with environmental hydrogen embrittlement

The physical characteristics of stress corrosion cracking of titanium in an aqueous chloride environment are compared with those of embrittlement of titanium by a gaseous hydrogen environment in an effort to help contribute to the understanding of the possible role of hydrogen in the complex stress corrosion cracking process. Based on previous studies, the two forms of embrittlement are shown to be similar at low hydrogen pressures (100 N/sq m) but dissimilar at higher hydrogen pressures. In an effort to quantify this comparison, tests were conducted in an aqueous chloride solution using the same material and test techniques as had previously been employed in a gaseous hydrogen environment. The results of these tests strongly support models based on hydrogen as the embrittling species in an aqueous chloride environment.

Nelson, H. G.↗

NASA NTRS1975

Embrittlement of nickel-, cobalt-, and iron-base superalloys by exposure to hydrogen

Five nickel-base alloys (Inconel 718, Udimet 700, Rene 41, Hastelloy X, and TD-NiCr), one cobalt-base alloy (L-605), and an iron-base alloy (A-286) were exposed in hydrogen at 0.1 MN/sq m (15 psi) at several temperatures in the range from 430 to 980 C for as long as 1000 hours. These alloys were embrittled to varying degrees by such exposures in hydrogen. Embrittlement was found to be: (1) sensitive to strain rate, (2) reversible, (3) caused by large concentrations of absorbed hydrogen, and (4) not associated with any detectable microstructural changes in the alloys. These observations are consistent with a mechanism of internal reversible hydrogen embrittlement.

Gray, H. R.↗

NASA NTRS1975

Analysis of liquid metal embrittlement from a bond energy viewpoint

Absorption induced embrittlement of solid metals by certain liquid metals is analyzed through an Engel-Brewer calculation of the solid-liquid interaction energy, and of the effect of the latter in reducing fracture surface energy. The reduction in fracture surface energy is estimated by comparison of the electronic contribution to the solid-liquid interaction energy with solid-solid bond energy for some 40 liquid-solid couples. Regular solution theory is used to estimate mutual solubility as the relative difference in parameter values. Embrittlement can be predicted by using reduction in fracture surface energy and solubility parameter difference as critical variables. The effect of solute additions to the liquid on the degree of embrittlement is interpreted via the same two variables; the principal effect of solutes is to modify solubility relationships at the solid-liquid interface.

Kelley, M. J.↗