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At least 19 records

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↗

Topological analysis of X-ray CT data for the recognition and trending of subtle changes in microstructure under material aging

X-ray computed tomography (CT) is an established non-destructive tool for 3D imaging of multiphasic composites. Numerous applications of X-ray CT in medical diagnosis and materials characterization have been reported, many involving field-specific innovations in the imaging technology itself. Yet, quantitative summarization to link image features to properties of interest has been rare. Here we address this issue by employing state-of-the-art technics in scalar field topology for the summarization of X-ray CT images of an example biphasic system. By varying processing-parameters we create different microstructures, evolve them through accelerated thermal aging, CT-image them pre- and post-aged, and demonstrate the ability of our image summarization method to systematically track process- and age-related changes, which can often be very subtle. A novel aspect of the algorithm involves recognition over multiple resolution levels, which provides deeper insight into the pattern relationship between grain-like features and their neighbors. The method is general, adaptable to diverse image reconstruction methods and materials systems, and particularly useful in applications where practical constraints on the sample-size limits the reliable use of more complex models, e.g., convolutional neural networks.

36 MATERIALS SCIENCE↗

Advanced In-situ Diagnostics for Multicomponent Gas Analysis and Material Aging Part 2: Compact Determination of Hydrogen Isotopes

This report has been accepted for publication in the journal Fusion Science and Technology, in the special issue associated with the Tritium 2016 conference, where the work was presented. Scanning calorimetry of a confined, reversible hydrogen sorbent material has been previously proposed as a method to determine compositions of unknown mixtures of diatomic hydrogen isotopologues and helium. Application of this concept could result in greater process knowledge during the handling of these gases. Previously published studies have focused on mixtures that do not include tritium. This paper focuses on modeling to predict the effect of tritium in mixtures of the isotopologues on a calorimetry scan. The model predicts that tritium can be measured with a sensitivity comparable to that observed for hydrogen-deuterium mixtures, and that under some conditions, it may be possible to determine the atomic fractions of all three isotopes in a gas mixture.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Age-aware materials model for foam cushions - considering time-dependence of strain-rates and rate-independent measurements

Over the last few reports we have chronicled the progressive development of an age-aware materials model for foam cushions relevant to our systems. The latest version employs a N = 2 Ogden Hyperfoam model within a two-network Tobolsky scheme. As the material ages, the first network progressively loses in strength, while the second network progressively gains in strength. However, the two networks are in different strain states. Thus, in additive equilibrium (Tobolsky model) they manifest both permanent structural changes (measured as Compression Set) as well as changes in mechanical strength and modulus (measured as Load Retention).

36 MATERIALS SCIENCE↗

Mechanical Properties of Aged A709

A709 plate is in the process of being developed and qualified through a collaboration by Argonne National Laboratory (ANL), Idaho National Laboratory (INL), and Oak Ridge National Laboratory (ORNL). The goal is to qualify A709 plate in Section III, Division 5 of the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code (BPVC). This would permit the construction of A709 plate for fast-reactor structural applications. A tradeoff between creep and creep-fatigue properties was established in prior work. A processing route was identified as providing the optimal balance between creep-rupture and elevated-temperature cyclic properties for the solution annealed condition. This condition, however, resulted in a shorter than desired creep-rupture life. Aging is probed to evaluate its potential at further improving mechanical properties. Aging statically precipitates the solutes in solution prior to service. The processing routes identified as providing the best creep-rupture properties and best balance in mechanical properties are investigated. This report discloses the results from tensile, creep, and elevated-temperature cyclic testing performed at INL on the aged material. The aged properties are compared to solution annealed properties. A709 offers improvement in performance compared to 316H particularly at high temperatures; 316H is a material qualified in Section III, Division 5 of the ASME BPVC. For certain high-temperature fast-reactor design conditions, 316H cannot be used while A709 can.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A review of predictive nonlinear theories for multiscale modeling of heterogeneous materials

Since the beginning of the industrial age, material performance and design have been in the midst of innovation of many disruptive technologies. Today's electronics, space, medical, transportation, and other industries are enriched by development, design and deployment of composite, heterogeneous and multifunctional materials. As a result, materials innovation is now considerably outpaced by other aspects from component design to product cycle. In this article, we review predictive nonlinear theories for multiscale modeling of heterogeneous materials. Deeper attention is given to multiscale modeling in space and to computational homogenization in addressing challenging materials science questions. Moreover, we discuss a state-of-the-art platform in predictive image-based, multiscale modeling with co-designed simulations and experiments that executes on the world's largest supercomputers. Such a modeling framework consists of experimental tools, computational methods, and digital data strategies. Once fully completed, this collaborative and interdisciplinary framework can be the basis of Virtual Materials Testing standards and aids in the development of new material formulations. Moreover, it will decrease the time to market of innovative products.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

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↗

The Nuclear Fuel Cycle: Safe Management of Spent Nuclear Fuel

The aim for storage of spent nuclear fuel (SNF) either in wet or in dry storage systems is to ensure general safety objective s are met throughout a desired storage period. Staff at the Savannah River National Laboratory (SRNL), in collaborations with partners at other national laboratories, industry research organizations, and the University of South Carolina (UofSC), have performed materials aging testing and analyses, and have established nuclear materials aging management programs to support extended periods of safe storage of research reactor (RR) SNF and of commercial power reactor (PR) SNF pending ultimate disposal. Several example challenges include susceptibility of aluminum SNF from research reactors to corrosion in poor quality water (wet storage). In dry storage, aluminum SNF can release hydrogen via radiolysis of the hydrated oxides on the aluminum cladding. Austenitic stainless steel canisters used for dry storage are susceptible to chloride-induced stress corrosion cracking (outside-in attack) that threaten the confinement boundary provided by the canister. This paper further describes these challenges, among others, and the formulated solutions to support extended safe storage of SNF.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

High-resolution setup for measuring wavelength sensitivity of photoyellowing of translucent materials

Polystyrene and many other materials turn yellow when exposed to ultraviolet (UV) radiation. All photodegradation mechanisms including photoyellowing are functions of the exposure wavelength, which can be described with an action spectrum. In this work, a new high-resolution transmittance measurement setup based on lasers has been developed for measuring color changes, such as the photoyellowing of translucent materials aged with a spectrograph. The measurement setup includes 14 power-stabilized laser lines between 325 nm and 933 nm wavelengths, of which one at a time is directed on to the aged sample. The power transmitted through the sample is measured with a silicon detector utilizing an integrating sphere. The sample is mounted on a high-resolution XY translation stage. Measurement at various locations aged with different wavelengths of exposure radiation gives the transmittance data required for acquiring the action spectrum. The combination of a UV spectrograph and the new high-resolution transmittance measurement setup enables a novel method for studying the UV-induced ageing of translucent materials with a spectral resolution of 3–8 nm, limited by the adjustable spectral bandwidth range of the spectrograph. These achievements form a significant improvement over earlier methods.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Dielectric and Mechanical Behavior of Thermally Aged EPR/CPE Cable Materials

Power and instrumentation cables play a crucial role in the safe operation of Nuclear Power Plants (NPPs). Thermal and other stressors present in the reactor environment cause the cable materials to degrade. In this work, dielectric and mechanical properties of cable insulation and jacket materials are studied as they are thermally aged, supporting development of non-destructive evaluation sensors for monitoring cable aging. Materials selected for this study are found in certain types of single-core unshielded power cables. These utilize ethylene propylene rubber (EPR)-based insulation material and chlorinated polyethylene (CPE)-based jacket material. Flat mats of these materials were obtained from the cable manufacturer and thermally aged at 140 °C in an air-circulating oven. Elongation-at-break was measured on tensile specimens stamped from the aged mats, and dielectric properties were measured from 100 Hz to 100 kHz using a parallel plate capacitor and precision LCR meter. In the case of aged EPR-based materials, rapid decrease in elongation at break indicating end of useful life was accompanied by a significant increase in dissipation factor, D, measured at 100 kHz. Capacitive measurement of D shows promise, therefore, as a non-destructive indicator of corresponding mechanical property changes in thermally-aged EPR-based insulation materials.

cable aging, nuclear cables, material degradation,↗

Effects of Eta Phase on Creep Performance of the Nickel-Base Superalloy 263

In wrought nickel-base alloys used at elevated temperatures for extended periods of time, it is commonly observed that unwanted phases may nucleate and grow. One such phase is the eta phase, based on Ni3Ti, which is a plate-shaped precipitate that nucleates at the grain boundaries and grows at the expense of the strengthening gamma prime phase. In order to study the effects of eta phase on creep performance, Alloy 263 was modified to contain 3 different microstructures: standard (contains gamma prime); aged (contains gamma prime and eta); and modified (contains only eta and no gamma prime). These microstructures were then creep tested in the range of 973-1123 K (700-850°C). An extensive test matrix revealed that the eta-only modified alloy had creep rupture strengths within 10% of the standard alloy even though this alloy had no strengthening gamma prime precipitates. It also exhibited superior creep ductility. A preliminary test matrix on the aged material containing eta and gamma prime prior to the creep tests revealed that the performance of this microstructure was generally between that of the standard alloy (best) and the eta-only alloy (worst). The aged material exhibited far superior creep ductility. These results suggest that the presence of the eta phase may not be deleterious to creep ductility, and in fact, may enhance it.

36 MATERIALS SCIENCE↗