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At least 1,261 records · Page 70

Grain Growth and Precipitation Behavior of Iridium Alloy DOP-26 During Long Term Aging

The influence of long term aging on grain growth and precipitate sizes and spatial distribution in iridium alloy DOP-26 was studied. Samples of DOP-26 were fabricated using the new process, recrystallized for 1 hour (h) at 1375 C, then aged at either 1300, 1400, or 1500 C for times ranging from 50 to 10,000 h. Grain size measurements (vertical and horizontal mean linear intercept and horizontal and vertical projection) and analyses of iridium-thorium precipitates (size and spacing) were made on the longitudinal, transverse, and rolling surfaces of the as-recrystallized and aged specimens from which the two-dimensional spatial distribution and mean sizes of the precipitates were obtained. The results obtained from this study are intended to provide input to grain growth models.

36 MATERIALS SCIENCE↗

Report on Aging and Irradiation Theoretical Model Development for Alloy 690 in Grizzly

This report describes the current efforts to implement a model to predict the engineering scale behavior of irradiated and aged Ni 2 Cr model alloy and Alloy 690 into the Grizzly software. Grizzly is a multiphysics simulation code under development at Idaho National Laboratory to simulate aging mechanisms and their effects on the integrity of critical LWR components. Engineering scale behavior of materials are strongly impacted by the underlying microstructure: the distribution and interaction of dislocations and defects within the individual grains dictates how the material will respond to loading. The evolution of these dislocations and defects determines how the engineering scale material will perform under different loading and environmental conditions. Mesoscale models can function as a bridge to connect microstructure evolution models to engineering models of the ductile-brittle transition temperature (DBTT) curve and fracture. The toughness of a material, which governs the engineering scale fracture behavior, is a function of both elastic deformation and plastic deformation. While the yield stress measurements capture the elastic contribution to a material’s toughness, information about the dislocation movement is required to understand the plastic component of toughness. Crystal plasticity models predict dislocation density evolution and thereby connect microstructure evolution to engineering scale behavior predictions. These models calculate the plastic strain within a metal as a function of dislocations and other crystal defects, including precipitates and interstitial loops, among others, by tracking dislocation movement and the interaction of these dislocations with the crystal defects. Within NiCr alloys, long-range ordered (LRO) precipitates form under aging conditions. These precipitates act as barriers to dislocation motion and are either sheared by dislocations or pin dislocations. Additional defects, such as stacking fault tetrahedra (SFTs) from irradiation damage, also impede dislocation motion in these alloys. A crystal plasticity mode for Ni 2 Cr model alloy and Alloy 690 is being currently implemented in the Grizzly code at INL. This report includes a description of the theoretical models incorporated into the Grizzly crystal plasticity code. These theoretical models include mechanisms for dislocation glade and twinning as well as dislocation-defect interaction relationship for both LRO precipitates and SFTs. We have selected these dislocation models based on the deformation mechanisms observed in experimental micropillar compression tests conducted on the Ni 2 Cr model alloy. The models are then extended to Alloy 690 with ongoing parameter fitting.

36 MATERIALS SCIENCE↗

Progress Summary: 12-Month Compression Set and Load Retention of Thermally Accelerated Aged Siloxane Specimens (Additively Manufactured by the Direct-Ink-Write (DIW) 3D Printing Technique) Was Measured

Motivation: Accelerated aging of polymeric materials is needed to predict their long-term mechanical functionality. Two key metrics used to evaluate their performance are compression set and load retention. A baseline(time=0)mechanical assessment was done prior to initiating the accelerated aging process to acquire initial thickness and load values for future calculation of compression set and load retention.Specimens are beingaged under compressive strain (13%for the current studies) at four different temperatures (25, 40, 55, and 70°C) for at least 1 year; compression set and load retention will be measured at various timepoints. Time-temperature superposition (TTS) will be applied to the isothermal data to obtain long-term predictions. Significance: Compression set is increasing with time and temperature, as expected. The increasing compression set is accompanied by decreasing load retention.The relativelylow compression set indicates the material is performing well.In a previous aging study, the legacy S5370 RTV foam exhibited 40% relative compression set after 12 months at 70°C, which is more than twice that of the DIW material. Progress:Data has been acquired out to the 12-month timepoint. Relative compression set and load retention versus time are shown in Fig. 1.A technical issue with the method of measuring load retention was discovered and previously reported load retention values have been adjusted; the current load retention values are estimates. TTS predictions are shown in Fig. 2.

36 MATERIALS SCIENCE↗

Advanced In-situ Diagnostics for Multicomponent Gas Analysis and Material Aging

Current methods of detecting material aging rely heavily on accelerated aging studies expensive, bulky, and resource-hungry diagnostics. We are developing compact gas analysis methods based on sensor platforms such as quartz crystal microbalances (QCM), using nanoporous metals and Metal-Organic Frameworks (MOFs), which enhance sensitivity and impart selectivity to analytes. Targeted analytes are O2 and other volatile analytes. In FY16 we installed and tested a new QCM system coupled to a commercial gas mixing system. This instrumentation provides a new multi-use capability that: 1) allows evaluation of detection of novel materials to enable selective detection of volatile species relevant to Enhanced Surveillance; 2) accelerates development of new thin film deposition methods for depositing these materials on sensing devices; and 3) enables in-situ monitoring, with sub-monolayer sensitivity, of the interaction of volatile species with material surfaces subject to aging or corrosion.

36 MATERIALS SCIENCE↗

Assessment of AFM - KPFM and SSRM for Measuring and Characterizing Materials Aging Processes

Atomic Force Microscopy (AFM), in conjunction with Peak Force Kelvin Probe Force Microscopy (PF-KPFM) and Peak Force Scanning Spreading Resistance Microscopy (PF-SSRM), was used to assess changes on thin metal films that underwent accelerated aging. The AFM technique provides a relatively easy, non-destructive methodology that does not require high-vacuum facilities to obtain nanometer-scale spatial resolution of surface chemistry changes. Surface morphology, roughness, contact potential difference, and spreading resistance were monitored to qualitatively identify effects of aging-morphology changes and oxidation of Au, Al, Cu thin film standards as well as diffusion of CuAu and AlAu thin film stacks at 65C under dried nitrogen flow conditions. AFM PF-KPFM and PF-SSRM modes have been exercised, refined and have proven to be viable and necessary early aging detection tools.

36 MATERIALS SCIENCE↗

Aging and Lifetimes Milestone 7777, G.C. #4: Assess the ability of MRI to identify chemical and mechanical heterogeneity in polymers at various length scales

Polysiloxane foams utilized for stockpile applications experience changes over time induced by exposure to thermal, radiative, and mechanical stresses. The interplay of these stresses can lead to chemical and/or physical changes in the polymer, such as compression set and material degradation over time. Understanding the mechanisms of material aging and identifying material degradation prior to failure are critical in maintaining the integrity of the nuclear stockpile. Our prior work using solid-state NMR spectroscopy has shown that we can observe signatures of thermal, radiative, and mechanical aging of silicone elastomers using differences in NMR parameters such as relaxation (T1 and T2). However, most of our measurements have been on bulk samples and have only provided an average aging behavior of each sample. Here, we have used magnetic resonance imaging (MRI) to provide relaxation-weighted images that are a metric of structural heterogeneity (cross-link density) in polymers across multiple length scales. In addition, the larger sample size that can be accommodated in animal MRI scanners has the potential to make the technique adaptable to detecting heterogeneities whole parts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

LLNL FY22 Aging and Lifetimes Exit Criteria: Milestone 8119, GC#01

Polysiloxane foams utilized for stockpile applications experience changes over time induced by exposure to thermal, radiative, and mechanical stresses. The interplay of these stresses can lead to chemical and/or physical changes in the polymer, such as compression set and material degradation over time. Understanding the mechanisms of material aging and identifying material degradation prior to failure are critical in maintaining the integrity of the nuclear stockpile. Our prior work using solid-state NMR spectroscopy has shown that we can observe signatures of thermal, radiative, and mechanical aging of silicone elastomers using differences in NMR parameters such as relaxation (T1 and T2). However, most of our measurements have been on bulk samples and have only provided an average aging behavior of each sample. Here, we have used magnetic resonance imaging (MRI) to provide relaxation-weighted images that are a metric of structural heterogeneity (crosslink density) in polymers across multiple length scales. In addition, the larger sample size that can be accommodated in animal MRI scanners has the potential to make the technique adaptable to detecting heterogeneities in whole parts.

36 MATERIALS SCIENCE↗

A Progress Report for a 44-month Aging Study on Nitroplasticizer (NP) Stability – Summary of KF and TGA Results

In the past few years, a 44-month long aging experiment was conducted under various aging conditions. The properties of aged nitroplasticizer (NP) samples were analyzed using Fourier transform infrared spectroscopy, Karl Fischer (KF) titration, thermogravimetric analysis (TGA), liquid chromatography tandem quadrupole time of flight mass spectrometry, and ion chromatography. In this progress report, complete KF and TGA results are reported and discussed.

36 MATERIALS SCIENCE↗

A mechanistic model for creep and thermal aging in Alloy 709

This report describes a physics-based model for creep and thermal aging in Alloy 709. Alloy 709 is an advanced austenitic alloy, targeted for use in future Sodium Fast Reactors (SFRs) and other advanced reactors. The material has superior high temperature properties compared to currently qualified 316 and 304 stainless steels. However, the available creep and thermal aging test database for Alloy 709 is significantly more limited compared to the historical materials. The physics-based model developed here is one way to accelerate the qualification of the material by providing more accurate long-term predictions for creep properties and thermal aging, compared to current empirical time-extrapolate techniques. The crystal plasticity finite element model is used to predict the deformation and failure of alloy 709. The same setup for the CPFE model is used in both the baseline model calibration process and the simulation campaigns for parameter inference. Specific constitutive choices are made for Alloy 709 to capture the primary deformation mechanisms. The dislocation creep formulation developed by Hu and Cocks is extended to account for coupled precipitation formation and the grain boundary cavitation model developed by Sham, Needleman, et al. is used to model grain boundary cavitation-induced failure. A novel update algorithm is proposed to render the semi-discrete constitutive update for the Sham-Needleman model unconditionally stable. A progressive calibration approach is adopted based on the observations that several types of material responses can be effectively decoupled. A surrogate model is trained based on full-fledged CPFE simulations to accelerate the forward model evaluations, and stochastic variational inference (SVI) is used to calibrate the unknown microstructural model parameters. The calibrated mechanistic model is used to predict the long-term creep life of Alloy 709, and the predictions are compared against classical empirical approaches.

36 MATERIALS SCIENCE↗

LLNL FY23 Aging and Lifetimes Exit Criteria: Milestone 8650, GC #4

Silicone rubbers are important materials within the complex and are used in various applications due to wide operating temperatures, favorable aging characteristics, and chemical inertness. However, silicone rubbers are susceptible to degradation in the presence of acid or base. The goal of the project is to design outgassing vessels to probe material degradation byproducts from additively manufactured (AM) silicones compressed against Arrhenius base under dry (sub 100 ppm moisture) environments. The overarching goal of this task is to develop a mechanistic understanding of degradation from experimental data that will be used to inform predictive lifetime and aging models. An outgassing chamber for multi-material compressive aging was designed. The chamber consists of a stainless-steel enclosure, which is hermetically sealed once AM silicone samples are compressed against Arrhenius base pellets in compression rigs (Fig. 1). Outgassing chambers, compression rigs, and accessories were procured, arrived onsite, and received surface treatments. Outgassing of degradation byproducts will be monitored over 12 weeks at 35 °C and 70 °C.

36 MATERIALS SCIENCE↗

Fast Semi-automated Filtration Method for Non-targeted LC-QTOF Data of Aged Nitroplasticizer Samples

A full dataset of aged nitroplasticizer (NP) is composed of more than 2000 unique mass-to-charges (m/z) when combining the non-targeted data obtained from both positive and negative electrospray ionization modes in time-of-flight mass spectrometry. Therefore, manual processing of these data often takes days, weeks, or even months to scrutinize for mechanistic insights. To effectively extract meaningful signals that represent vital degradation intermediates in the early NP degradation mechanism, a semi-automated postprocessing workflow for data filtering, tailored to the aging experiment of NP, has been developed. The automated portion of this workflow is written in a Python code (using pandas, numpy, and matplotlib libraries), which removes more than 65% of potential false signals within seconds via four threshold-based adjustable filters: signal sensitivity, coefficient of variation, number of measurements, and retention time variability. As for the manual portion, a pattern-based inspection method is employed to reduce another 23% or more false positives, which greatly simplifies data visualization and results in less than 3% of potential candidate m/z needing in-depth data interpretation. As a positive control, known compounds are verified. Using this semi-automated data reduction method, the amount of time required is reduced to a matter of hours for data filtering in the non-targeted datasets of aged NP, which saves more time and effort for compound identification.

36 MATERIALS SCIENCE↗

Accelerated Aging Scoping Study of Additively Manufactured Coupons

Additive manufacturing (AM) is a relatively new technological advancement that allows for rapid prototyping, development of intricate shapes, and reduction in manufacturing time. The materials of interest for this project are Ultem 1010, ABS M30, FDM Nylon 12, PC, and PPSF. However, little is known regarding the aging behavior of these AM materials. The limited aging study outlined herein was designed to compare the chemical, physical, and mechanical properties of AM parts as they experience accelerated aging at 70 °C for a total of 24 weeks. In general, ABS M30 stood out as it appeared to undergo chemical and physical changes leading to increase in density and an overall more brittle material, making this commonly used material not attractive for long-term use.

36 MATERIALS SCIENCE↗

Early Stages of Age Hardening in U-6%Nb: An Energy Barrier Hypothesis for Twin Reorientation

It is well known that age hardening occurs in U-6%Nb (Ref. 1-9). Figure 1 shows that increases in hardness occur at aging temperatures up to ~400°C, and overaging occurs above ~450°C. Overaging occurs by cellular decomposition of the αʺ b martensite, similar to overaging reactions in other uranium alloys. But the mechanism of age hardening remains elusive, particularly in its early stages.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

MOSAIC: An Effective FFT-based Numerical Method to Assess Aging Properties of Concrete

As the nuclear fleet in the United States ages and subsequent license renewal applications grow, the prediction of concrete durability at extended operation becomes more important. To address this issue, a Fast-Fourier Transform (FFT) method is utilized to simulate aging-related degradation of concrete within the Microstructure Oriented Scientific Analysis of Irradiated Concrete (MOSAIC) software. MOSAIC utilizes compositional phase maps to simulate damage from radiation-induced volumetric expansion (RIVE), applied force, creep, and thermal expansion. This compositional detail allows each mineral in the microstructure to be assigned specific material properties, allowing the simulation to be as accurate and representative as possible. The principal goal of MOSAIC is to simulate the effects of nonlinear aging mechanisms occurring in nuclear concrete on the macroscopic mechanical properties, using only the aggregate microstructure compositional information as a starting point. Here, several realistic example simulations are shown to demonstrate the utility and uniqueness of the MOSAIC software.

36 MATERIALS SCIENCE↗

Battery data integrity and usability: Navigating datasets and equipment limitations for efficient and accurate research into battery aging

A tremendous commitment of resources is needed to acquire, understand and apply battery data in terms of performance and aging behavior. There are many state of performance (SOP) and state of health (SOH) metrics that are useful to guide alignment of batteries to end-use, yet how these metrics are measured or extracted can make the difference between usable, valuable datasets versus data that lacks the necessary integrity to meet baseline confidence levels for SOP/SOH quantification. This work will speak to 1) types of data that support SOP and SOH evaluations on mechanistic terms, 2) measurement conditions needed to assure high data integrity, 3) equipment limitations that can compromise data high fidelity, and 4) the impact of cell polarization on data quality. A common goal in battery research and field use is to work from a data platform that supports economical paths of data capture while minimizing down-time for battery diagnostics. An ideal situation would be to utilize data obtained during normal daily use (“pulses or cycles of convenience”) without stopping the daily duty cycles to perform dedicated SOP/SOH diagnostic routines. However, difficulties arise in trying to make use of daily duty cycle data (denoted as cycle-by-cycle, CBC) that underscores the need for standardization of conditions: temperature and duty cycles can vary over the course of a day and throughout a week, month and year; polarization can develop within an immediate cycle and throughout successive cycles as a hysteresis. If CBC data is envisioned as a data source to determine performance and aging trends, it should be recognized that polarization is a frequent consequence of CBC and thus makes it difficult to separate reversible and irreversible components to metrics such as capacity loss and resistance increase over aging. Since CBC conditions can have a major impact on data usability, we will devote part of this paper to CBC data conditioning and management. Differential analyses will also be discussed as a means to detect changing trends in data quality. Our target cell chemistries will be lithium-ion types NMC/graphite and LMO/LTO.

25 ENERGY STORAGE↗

Relationship Between Filler Type, Thermomechanical Properties, and Aging of RTV Silicone Foams

Room-temperature vulcanizing (RTV) silicone foams are used in many industrial applications that require the material to perform over long time periods. However, mechanical properties tend to deteriorate when these foams age under a compressive load. The chemical aging is attributed to the presence of unreacted functional groups of the prepolymers, residues from acid, and catalytically active tin (II) species. Here, an optimized thermal treatment of an RTV foam that achieves completion of curing reactions and deactivation of reactive species is proposed. Foams that were thermally aged for three months under compressive load showed no signs of compression set, indicative of the effectiveness of the implemented post-curing approach. In addition, the effects of fillers (diatomaceous earth, fumed silica, and carbon nanofibers) on thermomechanical properties were investigated. Tensile strength, tear strength, and thermal conductivity increased when these fillers were added to the unfilled RTV formulation, with carbon nanofibers (CNFs) being the most effective filler. Rheological studies of RTV formulations indicated that 2.5 wt.% of CNFs is the upper limit that can be added to the RTV formulation.

36 MATERIALS SCIENCE↗

Seafood consumption among pregnant and non-pregnant women of childbearing age in the United States, NHANES 1999–2006

Objectives: Long-chain polyunsaturated fatty acids found in seafood are essential for optimal neurodevelopment of the fetus. However, concerns about mercury contamination of seafood and its potential harm to the developing fetus have created uncertainty about seafood consumption for pregnant women. We compared fish and shellfish consumption patterns, as well as their predictors, among pregnant and non-pregnant women of childbearing age in the US. Methods: Data from 1,260 pregnant and 5,848 non-pregnant women aged 1649 years from the 1999 to 2006 National Health and Nutrition Examination Survey (NHANES) were analyzed. Frequency and type of seafood consumed and adjusted associations of multiple characteristics with seafood consumption were estimated for pregnant and non-pregnant women, separately. Time trends were also examined. Results: There were no significant differences in the prevalence of fish or shellfish consumption, separately or combined, between pregnant and non-pregnant women using either the 30-day questionnaire or the Day 1, 24-h recall. Seafood consumption was associated with higher age, income, and education among pregnant and non-pregnant women, and among fish consumers these groups were more likely to consume ]3 servings in the past 30 days. Tuna and shrimp were the most frequently reported fish and shellfish, respectively, among both pregnant and non-pregnant women. We observed no significant time trends. Conclusion: There were no differences in seafood consumption between pregnant and non-pregnant women, and the factors related to seafood consumption were similar for both groups. Our data suggest that many women consume less than the recommended two servings of seafood a week.

59 BASIC BIOLOGICAL SCIENCES↗

THE LEECH EXOPLANET IMAGING SURVEY: ORBIT AND COMPONENT MASSES OF THE INTERMEDIATE-AGE, LATE-TYPE BINARY NO UMa

We present high-resolution Large Binocular Telescope LBTI/LMIRcam images of the spectroscopic and astrometric binary NO UMa obtained as part of the LBT Interferometer Exozodi Exoplanet Common Hunt exoplanet imaging survey. Our H-, K{sub s}-, and L′-band observations resolve the system at angular separations <0.″09. The components exhibit significant orbital motion over a span of ∼7 months. We combine our imaging data with archival images, published speckle interferometry measurements, and existing spectroscopic velocity data to solve the full orbital solution and estimate component masses. The masses of the K2.0 ± 0.5 primary and K6.5 ± 0.5 secondary are 0.83 ± 0.02 M{sub ⊙} and 0.64 ± 0.02 M{sub ⊙}, respectively. We also derive a system distance of d = 25.87 ± 0.02 pc and revise the Galactic kinematics of NO UMa. Our revised Galactic kinematics confirm NO UMa as a nuclear member of the ∼500 Myr old Ursa Major moving group, and it is thus a mass and age benchmark. We compare the masses of the NO UMa binary components to those predicted by five sets of stellar evolution models at the age of the Ursa Major group. We find excellent agreement between our measured masses and model predictions with little systematic scatter between the models. NO UMa joins the short list of nearby, bright, late-type binaries having known ages and fully characterized orbits.

79 ASTRONOMY AND ASTROPHYSICS↗