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All sourcesNASA NTRSDOE OSTI
NASA NTRS2014

Cosmic Ray Exposure Ages of Stony Meteorites: Space Erosion or Yarkovsky?

Space erosion from dust impacts may set upper limits on the cosmic ray exposure (CRE) ages of stony meteorites. A meteoroid orbiting within the asteroid belt is bombarded by both cosmic rays and interplanetary dust particles. Galactic cosmic rays penetrate only the first few meters of the meteoroid; deeper regions are shielded. The dust particle impacts create tiny craters on the meteoroid's surface, wearing it away by space erosion (abrasion) at a particular rate. Hence a particular point inside a meteoroid accumulates cosmic ray products only until that point wears away, limiting CRE ages. The results would apply to other regolith-free surfaces in the solar system as well, so that abrasion may set upper CRE age limits which depend on the dusty environment. Calculations based on N. Divine's dust populations and on micrometeoroid cratering indicate that stony meteoroids in circular ecliptic orbits at 2 AU will record 21Ne CRE ages of approx.176 x 10(exp 6) years if dust masses are in the range 10(exp -21) - 10(exp -3) kg. This is in broad agreement with the maximum observed CRE ages of approx. 100 x 10(exp 6) years for stones. High erosion rates in the inner solar system may limit the CRE ages of Near-Earth Asteroids (NEAs) to approx. 120 x 10(exp 6) years. If abrasion should prove to be approx. 6 times quicker than found here, then space erosion may be responsible for many of the measured CRE ages of main belt stony meteorites. In that case the CRE ages may not measure the drift time to the resonances due to the Yarkovsky effects as in the standard scenario, and that for some reason Yarkovsky is ineffective.

Yarkovsky↗
NASA NTRS2020

Spatial U-Pb Age Distribution in Shock-Recrystallized Zircon – A Case Study from the Rochechouart Impact Structure, France

Age determination of impact structures via the zircon U–Pb system remains challenging and often ambiguous due to highly variable effects of shock metamorphism on U-Pb geochronology. It is, therefore, crucial to link the observed zircon microtextures, including their temperature and pressure conditions associated with their formation, directly to the U–Pb ages preserved. Here, we analyzed three recrystallized zircon grains and one plastically deformed zircon crystal from the medium-sized Rochechouart impact structure in the northwestern Massif Central of France. For the Rochechouart impact structure the impact age (206.92 ± 0.32 Ma [40Ar/39Ar]) as well as the 2 tectono-themal history is well established making this study site ideal to test concepts about U-Pb systematics in shocked zircon and to differentiate between shock-driven age resetting and preimpact crystallization and metamorphic overprinting. Zircon microstructures were studied using scanning electron imaging, cathodoluminescence imaging, and electron backscatter diffraction (EBSD) mapping. Further, we conducted U–Pb Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) depth-profiling analysis, allowing us to interpret the resultant age data in discrete steps with increasing ablation time/depth. The U–Pb depth profiling data demonstrate that plastically strained grains are incompletely reset and preserve rim and interior age domains reflecting typical pre-impact (pre-Variscan and Variscan) regional tectonic ages. Our results also reveal that the granular crystals encountered contain microstructural evidence for “former reidite in granular neoblastic” (FRIGN) zircon, reflecting both high-pressure (⩾30GPa) and high temperature (⩾1200℃) conditions. This signifies that FRIGN zircon is now known from an additional, medium sized, impact structure further supporting the hypothesis that this impact induced microstructure is commonly preserved. In addition, FRIGN zircon has a high potential to preserve completely impact-reset crystal domains (~204 to 207 Ma) that can be identified by our combined analytical approach of U–Pb depth profiling and EBSD mapping, and thus are suitable for determining reliable impact ages

U-Pb depth profiling↗
DOE OSTI2014

Age-dependent changes in diastolic Ca{sup 2+} and Na{sup +} concentrations in dystrophic cardiomyopathy: Role of Ca{sup 2+} entry and IP{sub 3}

Highlights: • Age-dependent increase in [Ca{sup 2+}]{sub d} and [Na{sup +}]{sub d} in mdx cardiomyocytes. • Gadolinium significantly reduced both [Ca{sup 2+}]{sub d} and [Na{sup +}]{sub d} at all ages. • IP{sub 3}-pathway inhibition reduced cations concentrations in dystrophic cardiomyocytes. - Abstract: Duchenne muscular dystrophy (DMD) is a lethal X-inherited disease caused by dystrophin deficiency. Besides the relatively well characterized skeletal muscle degenerative processes, DMD is also associated with a dilated cardiomyopathy that leads to progressive heart failure at the end of the second decade. The aim of the present study was to characterize the diastolic Ca{sup 2+} concentration ([Ca{sup 2+}]{sub d}) and diastolic Na{sup +} concentration ([Na{sup +}]{sub d}) abnormalities in cardiomyocytes isolated from 3-, 6-, 9-, and 12-month old mdx mice using ion-selective microelectrodes. In addition, the contributions of gadolinium (Gd{sup 3+})-sensitive Ca{sup 2+} entry and inositol triphosphate (IP{sub 3}) signaling pathways in abnormal [Ca{sup 2+}]{sub d} and [Na{sup +}]{sub d} were investigated. Our results showed an age-dependent increase in both [Ca{sup 2+}]{sub d} and [Na{sup +}]{sub d} in dystrophic cardiomyocytes compared to those isolated from age-matched wt mice. Gd{sup 3+} treatment significantly reduced both [Ca{sup 2+}]{sub d} and [Na{sup +}]{sub d} at all ages. In addition, blockade of the IP{sub 3}-pathway with either U-73122 or xestospongin C significantly reduced ion concentrations in dystrophic cardiomyocytes. Co-treatment with U-73122 and Gd{sup 3+} normalized both [Ca{sup 2+}]{sub d} and [Na{sup +}]{sub d} at all ages in dystrophic cardiomyocytes. These data showed that loss of dystrophin in mdx cardiomyocytes produced an age-dependent intracellular Ca{sup 2+} and Na{sup +} overload mediated at least in part by enhanced Ca{sup 2+} entry through Gd{sup 3+} sensitive transient receptor potential channels (TRPC), and by IP{sub 3} receptors.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2016

Effect of cold rolling on microstructure and mechanical property of extruded Mg–4Sm alloy during aging

Microstructure and mechanical properties of the Mg–4Sm (wt.%) alloy, prepared via combined processes of extrusion, cold rolling and aging, have been investigated. The hot extruded alloy exhibits a weak rare earth magnesium alloy texture with < 11 − 21 >//ED, while the cold-rolled alloy shows a stronger basal texture with < 0001 >//ND. Many tensile twins and double twins are observed in grains after rolling. The cold-rolled alloy shows a weak age-hardening response compared with the extruded alloy, which is the result of more precipitation in the twin boundary during aging. The rolled alloy exhibits almost no precipitate free zone during aging compared with the extruded alloy. The higher proof stress of the rolled alloy in peak-aged condition is attributed to the presence of twin boundaries, stronger basal texture, higher dislocation density, and the suppression of precipitate free zone compared with the extruded alloy. - Highlights: • No precipitate free zone appears in cold-rolled alloy after aging. • Segregation and precipitates are observed in twin boundaries and grain boundaries. • Cold-rolled alloy shows a weak age-hardening response.

36 MATERIALS SCIENCE↗
DOE OSTI2015

GRIZZLY Model of Multi-Reactive Species Diffusion, Moisture/Heat Transfer and Alkali-Silica Reaction for Simulating Concrete Aging and Degradation

Concrete is widely used in the construction of nuclear facilities because of its structural strength and its ability to shield radiation. The use of concrete in nuclear power plants for containment and shielding of radiation and radioactive materials has made its performance crucial for the safe operation of the facility. As such, when life extension is considered for nuclear power plants, it is critical to have accurate and reliable predictive tools to address concerns related to various aging processes of concrete structures and the capacity of structures subjected to age-related degradation. The goal of this report is to document the progress of the development and implementation of a fully coupled thermo-hydro-mechanical-chemical model in GRIZZLY code with the ultimate goal to reliably simulate and predict long-term performance and response of aged NPP concrete structures subjected to a number of aging mechanisms including external chemical attacks and volume-changing chemical reactions within concrete structures induced by alkali-silica reactions and long-term exposure to irradiation. Based on a number of survey reports of concrete aging mechanisms relevant to nuclear power plants and recommendations from researchers in concrete community, we’ve implemented three modules during FY15 in GRIZZLY code, (1) multi-species reactive diffusion model within cement materials; (2) coupled moisture and heat transfer model in concrete; and (3) anisotropic, stress-dependent, alkali-silica reaction induced swelling model. The multi-species reactive diffusion model was implemented with the objective to model aging of concrete structures subjected to aggressive external chemical attacks (e.g., chloride attack, sulfate attack, etc.). It considers multiple processes relevant to external chemical attacks such as diffusion of ions in aqueous phase within pore spaces, equilibrium chemical speciation reactions and kinetic mineral dissolution/precipitation. The moisture/heat transfer module was implemented to simulate long-term spatial and temporal evolutions of the moisture and temperature fields within concrete structures at both room and elevated temperatures. The ASR swelling model implemented in GRIZZLY code can simulate anisotropic expansions of ASR gel under either uniaxial, biaxial and triaxial stress states, and can be run simultaneously with the moisture/heat transfer model and coupled with various elastic/inelastic solid mechanics models that were implemented in GRIZZLY code previously. This report provides detailed descriptions of the governing equations, constitutive equations and numerical algorithms of the three modules implemented in GRIZZLY during FY15, simulation results of example problems and model validation results by comparing simulations with available experimental data reported in the literature. The close match between the experiments and simulations clearly demonstrate the potential of GRIZZLY code for reliable evaluation and prediction of long-term performance and response of aged concrete structures in nuclear power plants.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
NASA NTRS2003

Aging of microstructural compartments in human compact bone

Composition of microstructural compartments in compact bone of aging male subjects was assessed using Raman microscopy. Secondary mineralization of unremodeled fragments persisted for two decades. Replacement of these tissue fragments with secondary osteons kept mean composition constant over age, but at a fully mineralized limit. Slowing of remodeling may increase fracture susceptibility through an increase in proportion of highly mineralized tissue. In this study, the aging process in the microstructural compartments of human femoral cortical bone was investigated and related to changes in the overall tissue composition within the age range of 17-73 years. Raman microprobe analysis was used to assess the mineral content, mineral crystallinity, and carbonate substitution in fragments of primary lamellar bone that survived remodeling for decades. Tissue composition of the secondary osteonal population was investigated to determine the composition of turned over tissue volume. Finally, Raman spectral analysis of homogenized tissue was performed to evaluate the effects of unremodeled and newly formed tissue on the overall tissue composition. The chemical composition of the primary lamellar bone exhibited two chronological stages. Organic matrix became more mineralized and the crystallinity of the mineral improved during the first stage, which lasted for two decades. The mineral content and the mineral crystallinity did not vary during the second stage. The results for the primary lamellar bone demonstrated that physiological mineralization, as evidenced by crystal growth and maturation, is a continuous process that may persist as long as two decades, and the growth and maturation process stops after the organic matrix becomes "fully mineralized." The average mineral content and the average mineral crystallinity of the homogenized tissue did not change with age. It was also observed that the mineral content of the homogenized tissue was consistently greater than the osteons and similar to the "fully mineralized" stage of primary bone. The results of this study demonstrated that unremodeled compartments of bone grow older through maturation and growth of mineral crystals in a protracted fashion. However, the secondary osteonal remodeling impedes this aging process and maintains the mean tissue age fairly constant over decades. Therefore, slowing of remodeling may lead to brittle bone tissue through accumulation of fully mineralized tissue fragments.

Non-NASA Center↗
DOE OSTI2015

Differential regulation of apoptosis in slow and fast twitch muscles of aged female F344BN rats

Age-related muscle atrophy is characterized by decreases in muscle mass and is thought be mediated, at least in part, by increases in myocyte apoptosis. Recent data has demonstrated that the degree of muscle loss with aging may differ between males and females while other work has suggested that apoptosis as indicated by DNA fragmentation may be regulated differently in fast- and slow-twitch muscles. Herein, we investigate how aging affects the regulation of muscle apoptosis in the fast-twitch extensor digitorum longus (EDL) and slow-twitch soleus muscles of young (6-month), aged (26-month), and very aged (30-month) female Fischer 344/NNiaHSD × Brown Norway/BiNia (F344BN) rats. Tissue sections were stained with hydroethidium for ROS and protein extract was subjected to immunoblotting for assessing apoptotic markers. Our data suggest that decreases in muscle mass were associated with increased DNA fragmentation (TUNEL positive) and increases in reactive oxygen species (ROS) as determined by hydroethidium staining in both the EDL and soleus. Similar to our previous work using aged male animals, we observed that the time course and magnitude of changes in Bax, Bcl-2, caspase-3, caspase-9, and cleavage of α-fodrin protein were regulated differently between muscles. As a result, These data suggest that aging in the female F344BN rat is associated with decreases in muscle mass, elevations in ROS level, increased muscle cell DNA fragmentation, and alterations in cell membrane integrity and that apoptotic mechanisms may differ between fiber types.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2020

Palladium/Zeolite Low Temperature Passive NOx Adsorbers (PNA): Structure-Adsorption Property Relationships for Hydrothermally Aged PNA Materials

Zeolites with different framework structures (SSZ-13, ZSM-5, BEA) but similar Si/Al ratios and Pd loading (~1 wr%) were synthesized and evaluated as low temperature passive NOx adsorbers (PNA). These materials exhibit high NOx adsorption efficiency with atomically dispersed Pd the active adsorption site. Hydrothermal aging at 750 ºC for 16 hours in the presence of 10% water vapor in air resulted in the formation of PdO nanoparticles in all three samples as evidenced by high energy XRD. Hydrothermal aging of the small-pore Pd/SSZ-13 (Si/Al = 6), which contain ~100-90% atomically dispersed palladium ions, decreases its PNA performance only by ~10-20%. High-field solid state 27Al NMR studies on the fresh and aged samples substantiate dealumination and significant changes in the distribution of Al (and thus, Bronsted acid) sites after hydrothermal aging. FTIR measurements with NO probe molecule and titration of Bronsted acid sites with nitrosyl (NO+) ions further corroborate the 27Al NMR data. Because framework aluminum atoms are the anchoring sites for atomically dispersed Pd ions, their elution from the framework causes the loss of active atomically dispersed Pd species. Furthermore, with the aid of HAADF-STEM imaging and synchrotron XRD studies, we further confirm and visualize the fate of these Pd species – they agglomerate into PdO nanoparticles on the external surface of zeolite. Consequently, these changes lead to the decrease in PNA performance of these materials after hydrothermal aging. The thus formed agglomerates cannot be re-dispersed back to their ionic state due to the loss of framework Al T-sites and/or inherent stability of such large PdO particles. Our study clearly demonstrates that, unlike in previous studies that found increased PNA performance upon HTA , high temperatures hydrothermal aging of PNA materials that contain atomically dispersed Pd initially, results in a decrease in NOx storage efficiency due mostly to the formation of PdO agglomerates. However, we also highlight the high hydrothermal stability of predominantly atomically dispersed 1-3 wt% Pd/SSZ-13 (Si/Al = 6), whose performance decreases only marginally after prolonged hydrothermal aging at 750 ºC. Overall, this study shows that hydrothermally stable passive NOx materials can be prepared using small-pore SSZ-13 zeolite.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Absence of superoxide dismutase activity causes nuclear DNA fragmentation during the aging process

Highlights: • Aging process increases ROS accumulation. • Aging process increases DNA damage levels. • Absence of SOD activity does not cause DNA damage in young cells. • Absence of SOD activity accelerate aging and increase oxidative DNA damages during the aging process. - Abstract: Superoxide dismutases (SOD) serve as an important antioxidant defense mechanism in aerobic organisms, and deletion of these genes shortens the replicative life span in the budding yeast Saccharomyces cerevisiae. Even though involvement of superoxide dismutase enzymes in ROS scavenging and the aging process has been studied extensively in different organisms, analyses of DNA damages has not been performed for replicatively old superoxide dismutase deficient cells. In this study, we investigated the roles of SOD1, SOD2 and CCS1 genes in preserving genomic integrity in replicatively old yeast cells using the single cell comet assay. We observed that extend of DNA damage was not significantly different among the young cells of wild type, sod1Δ and sod2Δ strains. However, ccs1Δ mutants showed a 60% higher amount of DNA damage in the young stage compared to that of the wild type cells. The aging process increased the DNA damage rates 3-fold in the wild type and more than 5-fold in sod1Δ, sod2Δ, and ccs1Δ mutant cells. Furthermore, ROS levels of these strains showed a similar pattern to their DNA damage contents. Thus, our results confirm that cells accumulate DNA damages during the aging process and reveal that superoxide dismutase enzymes play a substantial role in preserving the genomic integrity in this process.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2017

Airborne polycyclic aromatic hydrocarbons trigger human skin cells aging through aryl hydrocarbon receptor

Accumulating evidence suggests that polycyclic aromatic hydrocarbons (PAH) which adsorbed on the surface of ambient air particulate matters (PM), are the major toxic compound to cause cardiovascular and respiratory diseases, even cancer. However, its detrimental effects on human skin cell remain unclear. Here, we demonstrated that SRM1649b, a reference urban dust material of PAH, triggers human skin cells aging through cell cycle arrest, cell growth inhibition and apoptosis. Principally, SRM1649b facilitated Aryl hydrocarbon receptor (AhR) translocated into nucleus, subsequently activated ERK/MAPK signaling pathway, and upregulated aging-related genes expression. Most important, we found that AhR antagonist efficiently revert the aging of skin cells. Thus our novel findings firstly revealed the mechanism of skin aging under PAH contamination and provided potential strategy for clinical application. - Highlights: • SRM1649b inhibited the proliferation and lead to cell cycle arrest in human skin cells. • SRM1649b promoted apoptosis of human skin cells and induced cell aging. • SRM1649b caused AhR translocation into nucleus and upregulated aging-related genes. • The expression of aging-related genes were inhibited by AhR antagonist.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2012

Possible Origin of Improved High Temperature Performance of Hydrothermally Aged Cu/Beta Zeolite Catalysts

The hydrothermal stability of Cu/beta NH3 SCR catalysts are explored here. In particular, this paper focuses on the interesting ability of this catalyst to maintain and even enhance high-temperature performance for the "standard" SCR reaction after modest (900 °C, 2 hours) hydrothermal aging. Characterization of the fresh and aged catalysts was performed with an aim to identify possible catalytic phases responsible for the enhanced high temperature performance. XRD, TEM and 27Al NMR all showed that the hydrothermally aging conditions used here resulted in almost complete loss of the beta zeolite structure between 1 and 2 hours aging. While the 27Al NMR spectra of 2 and 10 hour hydrothermally-aged catalysts showed significant loss of a peak associated with tetrahedrally-coordinated Al species, no new spectral features were evident. Two model catalysts, suggested by these characterization data as possible mimics of the catalytic phase formed during hydrothermal aging of Cu/beta, were prepared and tested for their performance in the "standard" SCR and NH3 oxidation reactions. The similarity in their reactivity compared to the 2 hour hydrothermally-aged Cu/beta catalyst suggests possible routes for preparing multi-component catalysts that may have wider temperature windows for optimum performance than those provided by current Cu/zeolite catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Calendar life of lithium metal batteries: Accelerated aging and failure analysis

Lithium metal batteries (LMBs) are prime candidates for next-generation energy storage devices characterized by their remarkable energy storage capabilities. Despite the importance of understating the calendar aging impacts in LMBs, cycle life and calendar life have received inconsistent attention across various research and development stages. For acceptance into an application, especially electric vehicles, batteries are required to have sufficient calendar life to ensure performance over the life of vehicles which often experience extended periods of inactivity. In this study, an in-depth exploration into the calendar aging of LMB (Li/ Li[Ni 0.8 Mn 0.1 Co 0.1 ]O 2 in pouch cell format) is conducted. Specifically, the impact of calendar aging factors, state-of-charge (SOC), temperature, pressure, and operating conditions (open-circuit voltage, OCV and constant voltage, CV) on the surface morphology and thickness change rate in lithium metal anode is investigated. Notably, the results show that storing LMB pouch cells at an OCV, 80 % SOC, 25 °C, and 10 psi external pressure leads to a <1% reduction in capacity over 18 months. The results also suggest routes which can be utilized in the future for accelerated aging without altering the primary degradation modes. The results also show an accelerated calendar aging at high temperatures (45 °C), 100 % SOC, and CV suggesting they may serve as key accelerated aging methods for future studies. During calendar aging, pressure mitigates dendrite growth and extends calendar life. In conclusion, the insights from this study reinforce the viability of LMBs as a compelling solution for addressing increased energy storage needs in real-world applications.

25 ENERGY STORAGE↗
DOE OSTI2018

Grain boundary precipitation phenomena in an alloy 33 (Cr-Fe-Ni-N) subjected to direct-aging treatments (700 °C and 900 °C)

Highlights: • Complex GB precipitation occurs in Alloy 33 upon aging at 700 °C: conventional and DP modes. At 900 °C only the former occurs. • Two types of DP colonies were observed at 700 °C: unidirectional/parallel and multidirectional/irregular precipitates. • X-ray micro analyses reveal that irregular DP products develop more than one precipitate phase within the same DP colony. - Abstract: Precipitation behavior of alloy 33 upon isothermally aging at 700 °C and at 900 °C was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray energy dispersive spectroscopy (XEDS). The name, alloy 33, reflects the quasi-equal atomic content of the base elements Fe, Ni and Cr close to 33%, with the addition of Mo and N. The most remarkable features of the microstructural evolution resulting from the aging heat treatments are described as follows: aging at 700 °C leads to homogeneous and heterogeneous grain boundary precipitation, where the discontinuous mode is dominant at this temperature. Conversely, the opposite behavior was observed when the alloy is aged at 900 °C: predominantly homogeneous precipitation together with grain boundary precipitation, however with rare evidence for discontinuous precipitation (DP), even after longer aging times. In the present study, the topology and content of the DP colonies generated by the combined effect of grain boundary migration diffusion and precipitation under isothermal aging at 700 °C were particularly investigated. A variety of morphological features were observed: mainly (1) classical-type microstructure with straight and parallel lamellar precipitates with regular interlamellar spacing and (2) another microstructure with irregular and complex DP colonies. According to our analytical electron microscopy observations, the latter shows that there are more than one precipitate phase within the same colony, which is new to the current theory and experimental evidence on this subject.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Non-isothermal creep aging behaviors of an Al-Zn-Mg-Cu alloy

Highlights: • A novel non-isothermal creep aging (NICA) process is proposed to improve sheet metal forming efficiency. • Appropriate heating-cooling rate is conducive to obtain desired creep deformation and material properties. • The time consumption in optimized NICA process is about half of that in conventional creep aging process. • In NICA, the precipitates formed in heating will be dissolved nearby the peak temperature and re-precipitated in cooling. - Abstract: To shorten production period and reduce manufacturing cost of high strength aluminum alloy integral panel components, a novel non-isothermal creep age forming (CAF) technology was developed. Taking an Al-Zn-Mg-Cu alloy as the case material, the non-isothermal creep aging (NICA) behavior and the conventional isothermal creep aging (ICA) behavior were comparatively investigated. The corresponding creep deformations, material performance variations and precipitate microstructure evolutions were studied by creep aging tests, mechanical property and corrosion resistance tests, and transmission electron microscope (TEM) and scanning electron microscope (SEM) characterizations. Unlike the ICA which contains short heating and cooling stages and long holding stage, the NICA only has heating and cooling stages, viz., the alloy is heated slowly and the cooling stage begins immediately when reaching the peak temperature. In the NICA process, the precipitates nucleate and grow up in the first half of heating stage, resulting in the reduction of creep rate and enhancement of mechanical strength. The coarsening of precipitates occurs in the second half of heating stage, elevating the creep rate and significantly improving the corrosion resistance. Nearby the peak temperature, the primary precipitates partially dissolve, and the creep rate, mechanical strength and corrosion resistance decrease. Distinctive from the ICA process, a secondary precipitation phenomenon takes place in the cooling stage of NICA, leading to the recovery of high mechanical strength. The higher heating-cooling rate (1 °C/min) is not beneficial to accumulating creep deformation in the shorter creep aging period, while the lower one (0.25 °C/min) causes the loss of mechanical strength due to the excessive dissolution of precipitates. The moderate heating-cooling rate (0.5 °C/min) can lead to larger creep deformation, better mechanical properties and more satisfactory corrosion resistances in the NICA treated alloy, reaching 87.0% of creep strain, 105.7% of yield strength and 97.9% of electric conductivity in the ICA treated alloy. It is worth noting that the time consumption of the optimal NICA process is only 52.9% of the ICA process.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Optimization of direct aging temperature of Ti free grade 300 maraging steel manufactured using laser powder bed fusion (LPBF)

Maraging steels are of interest to the tool and die industry owing to their high strength, toughness and machinability. Additive manufacturing technologies like laser powder bed fusion (LPBF) can result in a paradigm shift in the design of maraging steel tools. Here, the lack of precipitates, in combination with solute segregation and non-equilibrium microstructure in Grade 300 maraging steel fabricated via LPBF makes the steel amenable to strengthening via direct aging post fabrication instead of the conventional solution treatment and aging. In this study we have focused on optimizing the direct aging temperature for a Ti-free Grade 300 maraging steel fabricated via LPBF for two different aging times. Through strain hardening analysis and detailed microstructural characterization, we show that direct aging at a temperature of 440 °C for 6 h resulted in the best strength-ductility combination. Aging samples at a lower temperature or shorter time resulted in no strain hardening prior to necking as a result of lower fraction of reverted austenite, whereas aging samples at a higher temperature resulted in extensive recrystallization of martensite, coarsening of precipitates, and extensive austenite reversion, resulting in softening of the fabricated parts.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Influence of grain size on α' Cr precipitation in an isothermally aged Fe-21Cr-5Al alloy

Cr-rich α' precipitation during aging typically leads to hardening and accordingly embrittlement of FeCrAl alloys, which needs to be suppressed. The influence of grain size on α' precipitation was studied by aging coarse-grained (CG), ultra-fine grained (UFG), and nanocrystalline (NC) ferritic Kanthal-D [KD; Fe-21Cr-5Al (wt.%) alloy] at 450, 500 and 550 °C for 500 h. After aging at 450 and 500 °C, less hardening was observed in the UFG KD than in CG KD. Atom probe tomography indicated a lower number density and larger sized intragranular α' in the UFG versus the CG alloy. The smaller grain size and higher defect (vacancy and dislocation) density in the UFG KD facilitated diffusion and accordingly enhanced precipitation kinetics, leading to coarsening of precipitates, as well as saturation of precipitation at lower temperatures, as compared to those in CG KD. No hardening occurred in UFG and CG KD after aging at 550 °C, indicating that the miscibility gap is between 500 and 550 °C. NC KD exhibited softening after aging owing to grain growth. α' precipitation occurred in NC KD aged at 450 °C but not at 500 °C, indicating that miscibility gap is between 450 and 500 °C. Thus, the significantly smaller grain size in NC KD decreased the miscibility gap, as compared to that in CG and UFG KD. Finally, this is attributed to the absorption of vacancies by migrating grain boundaries during aging, suppressing α' nucleation and enhancing Cr solubility.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Coupled aging effects in nanofiber-reinforced siloxane foams

Here, this study investigates the combined effects of ionizing radiation and thermal treatments on the aging of siloxane foams containing small amounts of carbon nanofibers. Our siloxane foams were exposed to accelerated aging conditions for more than two years, resulting in very low dose rates. In addition, foams were aged under compressive load to evaluate the strength of the porous microstructure. Samples were characterized by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance spectroscopy (NMR), Mössbauer, mass spectroscopy, electron paramagnetic resonance spectroscopy (EPR), solvent swelling, imaging techniques, uniaxial compressive load testing and tear testing. No significant changes in thermal stability or chemistry of the accelerated aged foam were observed, although gas evolution was detected. Changes in crystallization levels at low temperatures, microstructure, and mechanical properties were observed for foams with and without carbon nanofibers. In particular, foams aged under compressive load showed irreversible deformation of the porous microstructure. This study demonstrates that aging effects were enhanced when thermal and radiolysis were coupled together and that the addition of carbon nanofibers did not improve aging effects.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Aging mechanisms of filled cross-linked polyethylene (XLPE) cable insulation material exposed to simultaneous thermal and gamma radiation

Thermal and simultaneous thermal and gamma radiation aging experiments were conducted on an industry grade cross-linked polyethylene (XLPE) cable insulation material, which is a composite material with XLPE as polymer matrix and various additives and fillers. Reverse engineering was conducted to identify and quantify the material composition given that this information was not revealed by the cable manufacture. Samples were then aged at temperatures of 60, 90, and 115 °C, exposed to gamma radiation for total doses of 0 to 324 kGy, and at dose rates of 0 to 540 Gy/h. Aging mechanisms were studied using various materials characterization techniques including pyrolysis gas chromatography mass spectrometry (Py-GCMS), differential scanning calorimetry (DSC), nuclear magnetic resonance spectroscopy (NMR), and gel-fraction tests. Results show that the flame-retardant components were decomposed into smaller molecules when the material was exposed to gamma radiation, while no changes were observed when the samples were aged thermally without gamma radiation. With exposure to gamma radiation, the crystalline phase of the XLPE were damaged by gamma radiation introducing defects in the crystals, resulting in smaller and less perfect crystals. The dominance of chain scission or chain reformation process largely depends on the chain mobility, which is decided by the aging temperature. Chain scission was seen to dominate when the material was exposed to gamma radiation at 60 °C. Chain cross-linking slightly dominated when the material was exposed to gamma radiation at 90 °C and became more dominant with exposure to gamma radiation at 115 °C. No significant change to the XLPE polymer matrix was observed when the samples were exposed to thermal aging without gamma radiation. Finally, antioxidant is more effective in protecting the XLPE polymer matrix under thermal aging, but less effective with sample exposure to gamma radiation.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗