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At least 1,189 records · Page 66
All sourcesNASA NTRSDOE OSTI
DOE OSTI2013

Application of isotopic labeling, and gas chromatography mass spectrometry, to understanding degradation products and pathways in the thermal-oxidative aging of Nylon 6.6

Nylon 6.6 containing 13 C isotopic labels at specific positions along the macromolecular backbone has been subjected to extensive thermal-oxidative aging at 138 °C for time periods up to 243 days. In complementary experiments, unlabeled Nylon 6.6 was subjected to the same aging conditions under an atmosphere of 18 O 2 . Volatile organic degradation products were analyzed by cryofocusing gas chromatography mass spectrometry (cryo-GC/MS) to identify the isotopic labeling. The labeling results, combined with basic considerations of free radical reaction chemistry, provided insights to the origin of degradation species, with respect to the macromolecular structure. A number of inferences on chemical mechanisms were drawn, based on 1) the presence (or absence) of the isotopic labels in the various products, 2) the location of the isotope within the product molecule, and 3) the relative abundance of products as indicated by large differences in peak intensities in the gas chromatogram. The overall degradation results can be understood in terms of free radical pathways originating from initial attacks on three different positions along the nylon chain which include hydrogen abstraction from: the (CH 2 ) group adjacent to the nitrogen atom, at the (CH 2 ) adjacent the carbonyl group, and direct radical attack on the carbonyl. Understanding the pathways which lead to Nylon 6.6 degradation ultimately provides new insight into changes that can be leveraged to detect and reduce early aging and minimize problems associated with material degradation.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Long-term thermal aging of parylene conformal coating under high humidity and its effects on tin whisker mitigation

Usage of pure tin (Sn) or Sn-rich alloy in electronics industry is growing, which makes them more susceptible to the spontaneous growth of tin whiskers. The risk of having these whiskers can be dramatically mitigated by applying a conformal coating provided that it not only possesses excellent mechanical and adhesion properties but also maintains these properties throughout their service. Parylene C is commonly used as a conformal coating because of its favorable mechanical and physical properties, as well as superior conformal coverage. The purpose of this paper is to investigate the degradation of parylene C coating during the thermal aging in high humidity environment (85°C/85% relative humidity for up to 5000hrs) and its effect on the tin whisker mitigation capacity. It was observed that during aging at high temperature and high humidity (HTHH) environment, the oxidation occurs at early times, followed by bond scission, resulting in the loss of strength of the coating. Thinner parylene coating (12.5-μm-thick) had better coating adhesion on the silane-treated tin surface, so provided the better protection for tin whisker penetration than the thicker counterpart (25-μm-thick). After 2500hrs of aging, due to the degradation of the silane agent at the tin/parylene interface, the adhesion of the parylene coating was significantly weakened on the tin surface, which resulted in extensive corrosion of the tin solderpads. The loss of adhesion of the coating, along with the corrosion of the tin surface facilitated the tin whisker nucleation at the interface while the loss of mechanical strength and the brittleness made the coating easily penetrated by the growing whiskers. Tin whiskers with a smaller diameter were buckled and grew along the delaminated region while those with a larger diameter penetrated and continued to grow through the coating. Hence, the effectiveness of the parylene coatings on tin whisker mitigation is significantly reduced under long exposure to such high temperature and high humidity.

36 MATERIALS SCIENCE↗
DOE OSTI2014

In utero bisphenol A exposure disrupts germ cell nest breakdown and reduces fertility with age in the mouse

Bisphenol A (BPA) is a known reproductive toxicant in rodents. However, the effects of in utero BPA exposure on early ovarian development and the consequences of such exposure on female reproduction in later reproductive life are unclear. Thus, we determined the effects of in utero BPA exposure during a critical developmental window on germ cell nest breakdown, a process required for establishment of the finite primordial follicle pool, and on female reproduction. Pregnant FVB mice (F0) were orally dosed daily with tocopherol-striped corn oil (vehicle), diethylstilbestrol (DES; 0.05 μg/kg, positive control), or BPA (0.5, 20, and 50 μg/kg) from gestational day 11 until birth. Ovarian morphology and gene expression profiles then were examined in F1 female offspring on postnatal day (PND) 4 and estrous cyclicity was examined daily after weaning for 30 days. F1 females were also subjected to breeding studies with untreated males at three to nine months. The results indicate that BPA inhibits germ cell nest breakdown via altering expression of selected apoptotic factors. BPA also significantly advances the age of first estrus, shortens the time that the females remain in estrus, and increases the time that the females remain in metestrus and diestrus compared to controls. Further, F1 females exposed to low doses of BPA exhibit various fertility problems and have a significantly higher percentage of dead pups compared to controls. These results indicate that in utero exposure to low doses of BPA during a critical ovarian developmental window interferes with early ovarian development and reduces fertility with age. - Highlights: • In utero BPA exposure inhibits germ cell nest breakdown in female mouse offspring. • In utero BPA exposure alters expression of apoptosis regulators in the ovaries of mouse offspring. • In utero BPA exposure advances first estrus age and alters cyclicity in mouse offspring. • In utero BPA exposure causes various fertility problems in female mouse offspring.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2023

Northward propagation of the Gulf of Elat-Aqaba constrained by cosmogenic burial ages and magnetostratigraphy of onshore sediments

The Gulf of Elat-Aqaba (GEA), located in the southern part of the Dead Sea Transform (DST), is one of the most active segments of the Dead Sea fault system. Yet, some fundamental details concerning its evolution in space and time are still not fully understood. To better constrain the tectonic history of this region, we study a succession of alluvial, lacustrine, and fluvial deposits in the north-western edge of the GEA, which belong to the Quaternary Eilot and Garof Fms. The Eilot Fm. represents low-energy shallow freshwater bodies and sabkhas, which predate the development of the deep part of the basin. Later, in response to the subsidence of the basin, the Garof Fm. was deposited in alluvial fans that built up following the increase in the depositional energy. Cosmogenic burial ages combined with magnetostratigraphy show that these Fms. were deposited as early as 3.03 Ma and as late as 1.65 Ma, depending on the applied age model. Considering the present depth of the northern GEA, this age indicates a maximum subsidence rate of the head of the GEA of ~1.98mm/yr. We suggest that faults along the onshore margin of the deep basin were active during the deposition of the Garof Fm. and subsequently became inactive, while the faulting activity migrated toward the center of the basin. In conclusion, closed Holocene basins north of the present seashore, such as the Elat and Evrona playas, which may represent a modern analogue to the Plio-Pleistocene morphology, raise the possibility that the GEA head is still propagating northward.

58 GEOSCIENCES↗
DOE OSTI2018

Parameterized yields of semivolatile products from isoprene oxidation under different NOx levels: impacts of chemical aging and wall-loss of reactive gases

We developed a new parameterization for the yields of semi-volatile/intermediate volatility products from isoprene oxidation that took into account the chemical aging under different NOx levels, including functionalization and fragmentation reactions within the gas phase, oligomerization and photolysis within the condensed phase, as well as the loss of particles and gases to chamber walls. We used a box model to fit the dynamic evolution of measured secondary organic aerosol (SOA) concentrations from chamber experiments. The explicit inclusion of multigenerational gas phase chemistry and SOA oligomerization/photolysis during fitting itself had large impacts on the fitted yields that relate to the initial volatility distribution of isoprene oxidation products. During further multigenerational aging of these initial organics, we varied the branching ratio between functionalization and fragmentation. The best fits suggested increasing amounts of fragmentation with increasing initial NOx levels for mixed experiments. Using a box model to simulate evolution of SOA in the atmosphere at constant dilution rate (in absence of wall losses), we found that the yields determined by including different chemical scenarios during fitting changed predicted SOA mass concentrations substantially over aging timescale of 1-2 days. Our results demonstrated the need for better constraining smog-chamber-derived volatility distributions of both gas- and particle-phase SOA constituents with measurements.

Xing, Li↗
DOE OSTI2013

Excitation-emission spectra and fluorescence quantum yields for fresh and aged biogenic secondary organic aerosols

Certain biogenic secondary organic aerosols (SOA) become absorbent and fluorescent when exposed to reduced nitrogen compounds such as ammonia, amines and their salts. Fluorescent SOA may potentially be mistaken for biological particles by detection methods relying on fluorescence. This work quantifies the spectral distribution and effective quantum yields of fluorescence of SOA generated from two monoterpenes, limonene and a-pinene, and two different oxidants, ozone (O3) and hydroxyl radical (OH). The SOA was generated in a smog chamber, collected on substrates, and aged by exposure to ~100 ppb ammonia vapor in air saturated with water vapor. Absorption and excitation-emission matrix (EEM) spectra of aqueous extracts of aged and control SOA samples were measured, and the effective absorption coefficients and fluorescence quantum yields (~0.005 for 349 nm excitation) were determined from the data. The strongest fluorescence for the limonene-derived SOA was observed for excitation = 420+- 50 nm and emission = 475 +- 38 nm. The window of the strongest fluorescence shifted to excitation = 320 +- 25 nm and emission = 425 +- 38 nm for the a-pinene-derived SOA. Both regions overlap with the excitation-emission matrix (EEM) spectra of some of the fluorophores found in primary biological aerosols. Our study suggests that, despite the low quantum yield, the aged SOA particles should have sufficient fluorescence intensities to interfere with the fluorescence detection of common bioaerosols.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2022

“Did you eat a MOLEcule today?” An Interactive Demonstration of Molecular Weight with Real-Time Breath Analysis Using Mass Spectrometry for All Ages

Although mass spectrometry is a widely used analytical tool, age-appropriate, interactive outreach activities for laboratory visitors, especially children, are lacking. Furthermore, the presented interactive demonstration, “Did you eat a MOLEcule today?”, introduces all ages to molecular weight concepts and mass spectrometry in a research laboratory, while connecting the concepts to real-world applications. Through real-time breath analysis, participants explore the concepts of molecular weight, electrostatic field manipulation of charged molecules, and analyte identification by mass analysis. This module is rapid and highly adaptable for outreach activities but also includes age- or classroom-appropriate variations to decrease or increase difficulty levels. The presented interactive demonstration has repeatedly been implemented, with over 2300 participants during six annual “Take Our Daughters & Sons to Work Day” and two corporate “Family Day” outreach activities, successfully engaging, exciting, and educating both kids and parents.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Intrinsic Nanoscience of δ Pu-Ga Alloys: Local Structure and Speciation, Collective Behavior, Nanoscale Heterogeneity, and Aging Mechanisms

Because diffraction measurements are sensitive only to the long range average arrangement of the atoms in the coherent portion of a crystal, complementary local structure measurements are required for a complete understanding of the structure of a complex material. This is particularly an issue in solid solutions where even random distributions of a solute will result in nanometer-scale fluctuations in the local composition. The structure will be further complicated if collective and cooperative phenomena organize the solute distribution via longer range interactions between non-bonded solute sites. If the solute affects the phase stability then the question is raised of whether the atoms in domains with local compositions outside the limits of the bulk phase will rearrange into the structure stable for that composition and temperature or if the resulting stress would prevent such a local phase transition. If the former, then phase separated, heterogeneous structures at or below the diffraction limit will form. This nanometerscale competition between the phase transition and the epitaxial mismatch – exacerbated by the added strain if the transition involves a volume change – raises the potential for the formation of novel structures that do not occur in bulk material, e.g., fcc Fe. This coupling over multiple scales between inhomogeneity ordering, elastic forces, phase competition, and texture in the form of coexisting structures is a hallmark of martensites, a class of complex materials that includes δ-stabilized PuGa and that often exhibit correlated atomic and electronic properties. The enigmatic and extreme nature of Pu is consistent with its exhibiting unusual structural behavior of this type, including nanoscale heterogeneity in δ-stabilized PuGa and its enhanced homogeneity on aging that has been suggested based on earlier X-ray Absorption Fine Structure (XAFS) spectroscopy and x-ray pair distribution function (pdf) measurements. Measurements on a defined set of laboratory-prepared materials now corroborate and better describe this heterogeneity while additional aged samples demonstrate the role of heterogeneity in aging processes in Pu.

Conradson, Steven D.↗
DOE OSTI2021

Corrosion of lithium metal anodes during calendar ageing and its microscopic origins

Rechargeable lithium (Li) metal batteries must have long cycle life and calendar life (retention of capacity during storage at open circuit). Particular emphasis has been placed on prolonging the cycle life of Li metal anodes, but calendar ageing is less understood. Here, we show that Li metal loses at least 2–3% of its capacity after only 24 hours of ageing, regardless of the electrolyte chemistry. These losses of capacity during calendar ageing also shorten the cycle life of Li metal batteries. Cryogenic transmission electron microscopy shows that chemical corrosion of Li and the continuous growth of the solid electrolyte interphase—a passivation film on Li—cause the loss of capacity. Electrolytes with long cycle life do not necessarily form a solid electrolyte interphase with more resistance to chemical corrosion, so functional electrolytes must simultaneously minimize the rate of solid electrolyte interphase growth and the surface area of electrodeposited Li metal.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Mechanistic Understanding of Interphase-driven Aging in Silicon Anodes

Conventional solid electrolyte interphases (SEIs) strongly adhere to micro-silicon (µ-Si) and crack under volume changes, causing poor cycling performance. Nano-silicon improves cycling performance but remains costly with limited calendar life. Here potentiostatic ageing tests demonstrate that both calendar and cycle ageing are governed by SEI cracking and dissolution with different relative contributions. When the system is not dominated by SEI dissolution, the relative calendar life of Si anodes could correlates positively with their cycle life. LiF-rich SEI that enables long cycle life in µ-Si is therefore expected to enhance calendar life as well. Using this framework, we screened electrolytes, SEIs and electrodes and validated them with full-cell storage. LiF-rich SEI minimizes cracking and dissolution, enabling μ-Si to achieve excellent calendar life, whereas nano-silicon suffers from SEI dissolution and needs reduced electrolyte–electrode contact for better calendar life. This work clarifies calendar-ageing behaviour and accelerates electrolytes and SEI development for long-life Si anodes.

Johnson, Christopher S.↗
DOE OSTI2017

Human age and skin physiology shape diversity and abundance of Archaea on skin

The human skin microbiome acts as an important barrier protecting our body from pathogens and other environmental influences. Recent investigations have provided evidence that Archaea are a constant but highly variable component of the human skin microbiome, yet factors that determine their abundance changes are unknown. Here, we tested the hypothesis that the abundance of archaea on human skin is influenced by human age and skin physiology by quantitative PCR of 51 different skin samples taken from human subjects of various age. Our results reveal that archaea are more abundant in human subjects either older than 60 years or younger than 12 years as compared to middle-aged human subjects. These results, together with results obtained from spectroscopy analysis, allowed us gain first insights into a potential link of lower sebum levels and lipid content and thus reduced skin moisture with an increase in archaeal signatures. In conclusion, amplicon sequencing of selected samples revealed the prevalence of specific eury- and mainly thaumarchaeal taxa, represented by a core archaeome of the human skin.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2014

Complex refractive indices in the near-ultraviolet spectral region of biogenic secondary organic aerosol aged with ammonia

Atmospheric absorption by brown carbon aerosol may play an important role in global radiative forcing. Brown carbon arises from both primary and secondary sources, but the mechanisms and reactions for the latter are highly uncertain. One proposed mechanism is the reaction of ammonia or amino acids with carbonyl products in secondary organic aerosol (SOA). We generated SOA in situ by reacting biogenic alkenes (α-pinene, limonene, and α-humulene) with excess ozone, humidifying the resulting aerosol, and reacting the humidified aerosol with gaseous ammonia. We determined the complex refractive indices (RI) in the 360 – 420 nm range for these aerosols using broadband cavity enhanced spectroscopy (BBCES). The average real part (n) of the measured spectral range of the NH3-aged α-pinene SOA increased from n = 1.50 (±0.01) for the unreacted SOA to n = 1.57 (± 0.01) after a 1.5h exposure to 1.9 ppm NH3; whereas,the imaginary component (k) remained below k < 0.001 (± 0.002). For the limonene and α-humulene SOA the real part did not change significantly, and we observed a small change in the imaginary component of the RI. The imaginary component increased from k = 0.0 to an average k= 0.029 (± 0.021) for α-humulene SOA, and from k < 0.001 (± 0.002) to an average k = 0.032 (±0.019) for limonene SOA after a 1.5 h exposure to 1.3 and 1.9 ppm of NH3, respectively. Collected filter samples of the aged and unreacted α-pinene SOA and limonene SOA were analyzed off-line with nanospray desorption electrospray ionization high resolution mass spectrometry (nano-DESI/HR-MS), and in-situ with a Time-of-Fligh Aerosol Mass Spectrometer, confirming that the SOA reacted and that various nitrogen-containing reaction products formed. If we assume that NH3 aging reactions scale linearly with time and concentration, then a 1.5 h reaction with 1 ppm NH3 in the laboratory is equivalent to 24 h reaction with 63 ppbv NH3, indicating that the observed aerosol absorption will be limited to atmospheric regions with high NH3 concentrations.

20 refractive index↗
DOE OSTI2024

Aluminosilicate colloidal gels: from the early age to the precipitation of zeolites

Aluminosilicate hydrogels are often considered to be precursors for the crystallisation of zeolites carried out under hydrothermal conditions. The preparation of mechanically homogeneous aluminosilicate gels enables the study of these materials through bulk rheology and observation of the aging dynamics until the precipitation of crystalline zeolites. The first part of this study deals with the establishment of ternary state diagrams, in order to identify the range of chemical formulations that enable preparation of single-phase homogeneous gels. Then, by studying the viscoelastic moduli during the gelation reaction, and by yielding the gel under large deformation, we propose an empirical law considering the partial order of reaction on each chemical element, to predict the gelation time according to the chemical formulation. The scaling behavior of the elastic properties of this colloidal gel shows a transition from a strong link behavior to a weak link regime. Long term aging results in the shrinkage of the gel, accompanied by syneresis of interstitial liquid at the surface. Zeolites precipitate through crystallisation by a particle attachment mechanism, when thermodynamic equilibrium is reached. The stoichiometry of the precipitated zeolites is not only consistent with the concentration of the remaining species in the supernatant but, surprisingly, it is also very close to the partial order of the reaction of the chemical elements involved in the determination of the critical gel point. This indicates a strong correlation between the morphology of the soft amorphous gel network that is formed at an early age and those of the final solid precipitated crystals.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Star formation rate and stellar mass calibrations based on infrared photometry and their dependence on stellar population age and extinction

The stellar mass (M $\star$ ) and the star formation rate (SFR) are among the most important features that characterize galaxies. Measuring these fundamental properties accurately is critical for understanding the present state of galaxies, their history, and future evolution. Infrared (IR) photometry is widely used to measure the M $\star$ and SFR of galaxies because the near-IR traces the continuum emission of the majority of their stellar populations (SPs), and the mid/far-IR traces the dust emission powered by star-forming activity. This work explores the dependence of the IR emission of galaxies on their extinction, and the age of their SPs. It aims to provide accurate and precise IR-photometry SFR and M $\star$ calibrations that account for SP age and extinction while providing quantification of their scatter. We used the CIGALE spectral energy distribution (SED) fitting code to create model SEDs of galaxies with a wide range of star formation histories, dust content, and interstellar medium properties. We fit the relations between M $\star$ and SFR with IR and optical photometry of the model-galaxy SEDs with the Markov chain Monte Carlo (MCMC) method. As an independent confirmation of the MCMC fitting method, we performed a machine-learning random forest (RF) analysis on the same data set. The RF model yields similar results to the MCMC fits, thus validating the latter. This work provides calibrations for the SFR using a combination of the WISE bands 1 and 3, or the JWST NIR-F200W and MIRI-F2100W. It also provides mass-to-light ratio calibrations based on the WISE band-1, the JWST NIR-F200W, and the optical u - r or g - r colors. These calibrations account for the biases attributed to the SP age, while they are given in the form of extinction-dependent and extinction-independent relations. The proposed calibrations show robust estimations while minimizing the scatter and biases throughout a wide range of SFRs and stellar masses. The SFR calibration offers better results, especially in dust-free or passive galaxies where the contributions of old SPs or biases from the lack of dust are significant. Similarly, the M $\star$ calibration yields significantly better results for dusty and high-SFR galaxies where dust emission can otherwise bias the estimations.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2015

Age, Growth, and Reproduction in Two Coastal Populations of Longnose Gars

Abstract Measurements of age, growth, and reproduction are excellent tools for determining the ecological role and impact of a species within an ecosystem. Longnose Gar Lepisosteus osseus is a large, ubiquitous top predator in fresh and saline waters of the eastern United States. Even though the species is common, their basic biology has been largely uncharacterized in brackish and marine waters. Specimens were collected from two estuaries: Winyah Bay and Charleston Harbor, South Carolina, from May 2012 through July 2013 to examine age, growth, and reproduction in tidally influenced systems. This species is fairly long‐lived, with maximum ages of 17 and 25 years for males and females, respectively. The von Bertalanffy growth model yielded significantly higher growth rates for males than for females. Reproductive histology and the gonadosomatic index indicated that Longnose Gars exhibit determinate fecundity and spawn in late spring following a long development period during fall and winter. These life history parameters provide valuable insight into the basic biology of Longnose Gars and into how they function in estuarine environments. Further research on the precise timing and location of spawning movement, as well as daily movement patterns of this species, would provide a more comprehensive knowledge of Longnose Gar reproductive biology.

Smylie, Meredith↗
DOE OSTI2017

Age and Method of Release Affect Migratory Performance of Hatchery Steelhead

Abstract Hatchery programs that are designed to aid recovery of natural populations of anadromous salmonids, including steelhead Oncorhynchus mykiss, require locally derived, natural-origin broodstock. In such programs, achieving smoltification size thresholds may require extending hatchery rearing beyond age 1. We compared out-migration survival and travel rates of 142,990 PIT-tagged steelhead smolts released at age 1 (S1 rearing strategy) or age 2 (S2 rearing strategy) over five release years at Winthrop National Fish Hatchery (WNFH, Okanogan County, Washington). An S2 rearing cycle produced larger smolts with more uniform size distributions, resulting in higher survival during the first portion of their out-migration than for S1 smolts in three of the five release years. The S2 smolts migrated more rapidly to the ocean than S1 smolts in all years except 2011 and arrived in the Columbia River estuary 5.4 d earlier on average than the S1 smolts. The S1 steelhead that did not leave during the volitional release were subsequently forced from the hatchery to measure their survival. Nonvolitional S1 migrants were smaller and had survival rates that were 2.3–66.3 times lower than those of S1 steelhead that left WNFH on their own. The same was true for S2 steelhead, but the magnitude of the survival difference between volitional migrants and fish forced from the raceways was less variable and ranged from 2.5- to 4.6-fold. We conclude that S2 rearing can be a successful strategy for producing smolts from local natural-origin broodstock, with out-migration survival and travel times that are equivalent to or better than those of S1 smolts produced from nonlocal broodstock. Received July 25, 2016; accepted March 31, 2017 Published online May 31, 2017

Tatara, Christopher P.↗
DOE OSTI2020

Tritium Aging Effects on Fracture Toughness of Stainless Steel Weldments

The long-term embrittlement effects of tritium and decay helium on the structural properties of stainless steels have been studied for years at Savannah River to provide required data for establishing safe operating conditions and lifetimes of pressure vessels used to contain tritium gas. In this study, the fracture toughness properties of the longest-aged tritium-precharged stainless-steel base metals and weldments tested at Savannah River were measured and compared to earlier results. The fracture toughness values were the lowest recorded here for tritium-exposed stainless steel. As-forged and as-welded specimens were thermally precharging with tritium gas at 34.5 MPa and 623 K, then aged for up to 17 years to buildin decay helium prior to testing. ASTM J-Integral fracture mechanics analyses, transmission electron microscopy (TEM), and small angle neutron scattering (SANS) examinations were conducted to characterize the effects of tritium and its radioactive decay product, helium-3. Results show that the fracture toughness values were reduced to less than 2-4% of the as-forged values for specimens with more than 1300 appm helium from tritium decay. The trend of decreasing fracture toughness values with increasing helium content was consistent with earlier observations, and the data show that Type 304L stainless steel is more resistant to tritium-induced cracking than Type 21-6-9 stainless at similar decay helium levels. The fracture toughness properties of long-aged weldments were also affected, but the reductions were not as severe over time because weldments did not retain as much tritium as did the base metals. TEM observations were used to characterize the effects of decay helium bubbles on the deformation substructures, but nanometer-sized helium bubbles were not easily resolved because of high dislocation densities within the forged microstructures. SANS results are presented that suggest the technique can provide information on decay helium bubble size, spacing, and distribution in these steels.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Performance Restoration of a Tritium-Aged LaNi 4.25 Al 0.75 Sample

Hydride beds containing LaNi 4.25 Al 0.75 (LANA.75) are used to store significant quantities of tritium. These hydride beds have a limited service life due to radiolytic decay of tritium to 3He within the metal matrix. The crystal structure of the hydride is altered by trapped 3 He, which has a very low solubility in the metal. The altered structure induces the formation of a heel of trapped hydrogen isotopes and diminishes the reversible capacity of the hydride. With sufficient tritium exposure, the bed loses the ability to deliver 3He-free tritium, and replacement is needed. Demonstration of a means to regenerate tritium-aged LANA.75 in situ would delay or even eliminate the need to replace lanthanum nickel aluminum (LANA) hydride beds. This paper presents test results obtained during regeneration testing. The efficacy of regeneration testing was evaluated by comparing tritium desorption isotherms collected on the hydride before and after exposure to regeneration conditions. Testing was performed on a bench-scale tritium-aged LANA.75 sample that was previously isotopically exchanged (from tritium to deuterium), passivated, and recovered. Once transferred to a high-temperature test cell, the deuterium heel of the sample was isotopically exchanged with tritium, and a baseline desorption isotherm was collected for comparison purposes. The sample was then heated under vacuum, and comparative isotherms were gathered between regeneration evolutions. Shifts in isotherms show progressive improvements with higher-temperature exposure over the tritium-aged baseline. The heel was significantly reduced, and the reversible capacity of the hydride was essentially restored to near virgin values. For all tested conditions, the plateau pressure remained higher than virgin LANA.75.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗