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At least 595 records · Page 33

Interpolation and extrapolation of creep rupture data by the minimum commitment method. III - Analysis of multiheats

An outline is presented of approaches for treating multiheats on the basis of the focal point convergence method. The method has been employed in the case of two highly characterized multiheats, including a 304 stainless steel studied in Japan and a low alloy carbon steel studied in England. The method makes use of the same functional form for all materials. Only the constants are varied for each multiheat. Completely computerized procedures are employed for the determination of the constants. Once the basic analysis has been performed, the representation of various members in the same system is achieved by adding linear expressions of log stress, changing only two constants in the equations to represent a selected heat.

Manson, S. S.↗

Sampling Soil for Characterization and Site Description

The sampling scheme for soil characterization within the GLOBE program is uniquely different from the sampling methods of the other protocols. The strategy is based on an understanding of the 5 soil forming factors (parent material, climate, biota, topography, and time) at each study site, and how each of these interact to produce a soil profile with unique characteristics and unique input and control into the atmospheric, biological, and hydrological systems. Soil profile characteristics, as opposed to soil moisture and temperature, vegetative growth, and atmospheric and hydrologic conditions, change very slowly, depending on the parameter being measured, ranging from seasonally to many thousands of years. Thus, soil information, including profile description and lab analysis, is collected only one time for each profile at a site. These data serve two purposes: 1) to supplement existing spatial information about soil profile characteristics across the landscape at local, regional, and global scales, and 2) to provide specific information within a given area about the basic substrate to which elements within the other protocols are linked. Because of the intimate link between soil properties and these other environmental elements, the static soil properties at a given site are needed to accurately interpret and understand the continually changing dynamics of soil moisture and temperature, vegetation growth and phenology, atmospheric conditions, and chemistry and turbidity in surface waters. Both the spatial and specific soil information can be used for modeling purposes to assess and make predictions about global change.

Levine, Elissa↗

Method Development for Experimental Characterization of Dynamic Strength of Aluminum Structures

Space Flight Hardware (SFH) experiences intense vibratory loading during flight, which only lasts a few minutes. When determining the appropriate size of these components to withstand such loading without becoming damaged (plastically deforming or breaking), standard design practice is to assume that the peak dynamic loads are applied statically. In doing so, the resulting stress is compared against a material strength parameter obtained from a quasi-static experiment. Since the near-peak stresses are only experienced over a small fraction of time in reality, this approach leads to design conservatism that unnecessarily increases structural mass as well as the associated inefficiency and financial cost. In an effort to modernize engineering design standards to appropriately consider the higher practical strength of dynamically loaded structures, this overarching research project seeks to develop an experimental test procedure for quantifying the dynamic strength of metallic alloys as a function of excitation frequency. In the ideal case, the characterization test would include an in-situ method for monitoring the onset and progression of plastic deformation of the test specimen undergoing vibratory loading. These new tests are designed to be high intensity (forcing amplitude), short term (60 seconds at full amplitude), and cyclic in nature (sinusoidal excitation via attached stinger to an otherwise cantilevered beam). In addition, the initial metallic alloy under investigation is 6061 aluminum, due to its wide use and applicability for SFH. Thus far, the most promising monitoring method under development with live-capacity is to track hysteresis behavior of the beam from power dissipation trends, calculated via force (from transducer on excitation stinger) and velocity (measurements from Laser Doppler Vibrometer) data and work to distinguish between elastic and plastic features. As a key component of this ongoing method development, any pseudo-live indication of plasticity can be corroborated against the outcome of a pre-post assessment of damage via macroscopic evaluation of beam geometry (i.e. assessing any permanent change in the beam’s tip deflection). Support for experimental design decisions as well as dynamic strength data from tests with excitation frequencies of 10, 40, and 55 Hz will be discussed. This work contributes to the foundation for a new type of vibration-based characterization experiments and generates initial data on the functional strength of 6061 aluminum under the conditions considered. Keywords: vibrations, plastic deformation, aluminum

vibrations↗

In Situ Test Method for the Electrostatic Characterization of Lunar Dust

This paper serves to illustrate the testing methods necessary to classify the electrostatic properties of lunar dust using in situ instrumentation and the required techniques therein. A review of electrostatic classification of lunar simulant materials is provided as is its relevance to the success of future human lunar missions.

Buhler, C. R.↗

Contrastive Machine Learning with Gamma Spectroscopy Data Augmentations for Detecting Shielded Radiological Material Transfers

Data analysis techniques can be powerful tools for rapidly analyzing data and extracting information that can be used in a latent space for categorizing observations between classes of data. Machine learning models that exploit learned data relationships can address a variety of nuclear nonproliferation challenges like the detection and tracking of shielded radiological material transfers. The high resource cost of manually labeling radiation spectra is a hindrance to the rapid analysis of data collected from persistent monitoring and to the adoption of supervised machine learning methods that require large volumes of curated training data. Instead, contrastive self-supervised learning on unlabeled spectra can enhance models that are built on limited labeled radiation datasets. This work demonstrates that contrastive machine learning is an effective technique for leveraging unlabeled data in detecting and characterizing nuclear material transfers demonstrated on radiation measurements collected at an Oak Ridge National Laboratory testbed, where sodium iodide detectors measure gamma radiation emitted by material transfers between the High Flux Isotope Reactor and the Radiochemical Engineering Development Center. Label-invariant data augmentations tailored for gamma radiation detection physics are used on unlabeled spectra to contrastively train an encoder, learning a complex, embedded state space with self-supervision. A linear classifier is then trained on a limited set of labeled data to distinguish transfer spectra between byproducts and tracked nuclear material using representations from the contrastively trained encoder. The optimized hyperparameter model achieves a balanced accuracy score of 80.30%. Any given model—that is, a trained encoder and classifier—shows preferential treatment for specific subclasses of transfer types. Regardless of the classifier complexity, a supervised classifier using contrastively trained representations achieves higher accuracy than using spectra when trained and tested on limited labeled data.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Lamb Wave Stiffness Characterization of Composites Undergoing Thermal-Mechanical Aging

The introduction of new, advanced composite materials into aviation systems requires a thorough understanding of the long term effects of combined thermal and mechanical loading upon those materials. Analytical methods investigating the effects of intense thermal heating combined with mechanical loading have been investigated. The damage mechanisms and fatigue lives were dependent on test parameters as well as stress levels. Castelli, et al. identified matrix dominated failure modes for out-of-phase cycling and fiber dominated damage modes for in-phase cycling. In recent years, ultrasonic methods have been developed that can measure the mechanical stiffness of composites. To help evaluate the effect of aging, a suitably designed Lamb wave measurement system is being used to obtain bending and out-of-plane stiffness coefficients of composite laminates undergoing thermal-mechanical loading. The system works by exciting an antisymmetric Lamb wave and calculating the velocity at each frequency from the known transducer separation and the measured time-of-flight. The same peak in the waveforms received at various distances is used to measure the time difference between the signals. The velocity measurements are accurate and repeatable to within 1% resulting in reconstructed stiffness values repeatable to within 4%. Given the material density and plate thickness, the bending and out-of-plane shear stiffnesses are calculated from a reconstruction of the dispersion curve. A mechanical scanner is used to move the sensors over the surface to map the time-of-flight, velocity, or stiffnesses of the entire specimen. Access to only one side of the material is required and no immersion or couplants are required because the sensors are dry coupled to the surface of the plate. In this study, the elastic stiffnesses D(sub 11), D(sub 22), A(sub 44), and A(sub 55) as well as time-of-flight measurements for composite samples that have undergone combined thermal and mechanical aging for a duration of 10,000 hours are reported.

Seale, Michael D.↗

Raman structural studies of the nickel electrode

Raman spectroscopy is sensitive to empirically controlled nickel electrode structural variations, and has unique potential for structural characterization of these materials. How the structure relates to electrochemical properties is examined so that the latter can be more completely understood, controlled, and optimized. Electrodes were impregnated and cycled, and cyclic voltammetry is being used for electrochemical characterization. Structural variation was observed which has escaped detection using other methods. Structural changes are induced by: (1) cobalt doping, (2) the state of change or discharge, (3) the preparation conditions and type of buffer used, and (4) the formation process. Charged active mass has an NiOOH-type structure, agreeing with X-ray diffraction results. Discharged active mass, however, is not isostructural with beta-Ni(OH)2. Chemically prepared alpha phases are not isostructural either. A disordered structural model, containing point defects, is proposed for the cycled materials. This model explains K(+) incorporation. Band assignments were made and spectra interpreted for beta-Ni(OH)2, electrochemical NiOOH and chemically precipitated NiOOH.

Cornilsen, B. C.↗

Innovative Nuclear Materials Outboard-A Project Specimen Preparation Guide

The Innovative Nuclear Materials (INM) Program was recently established by the U.S. Department of Energy (DOE) to develop advanced material technologies for use in nuclear reactors. The INM program is presently focused on researching in-core non-fueled materials for application in fast spectrum nuclear reactors. The widespread deployment of fast reactors continues to be a prominent aspiration for advanced nuclear technology developers. However, companies working to license these reactors have no choice but to rely on historic material technologies since further optimization and advancement of these materials is impeded by the lack of fast neutron irradiation test facilities. INM-OA is a non-fueled drop-in experiment which will irradiate material specimens of interest to fast reactor applications. This experiment will be irradiated at Idaho National Laboratory (INL) in the Advanced Test Reactor (ATR) outboard-A (OA) position during normal and high temperature steady state (HTSS) cycles. It will include material specimens supplied by members of the INM program and will utilize a cadmium-lined basket to filter out incident thermal neutrons, thus simulating a faster neutron energy spectrum. Material specimens will undergo post-irradiation examination including microscopy and mechanical testing. In addition to absorption reactions, fast neutrons cause microstructural damage in materials by atom displacement, which can cause exacerbated changes in physical properties and behavior. Thus, the data obtained from the INM-OA experiment will be crucial for understanding the engineering-scale behavior of reactor materials. This document is intended for the Principal Investigators providing samples for this project. Topics included are a general description of the experiment, the irradiation experiment/capsule design, sample geometries, number of samples to be provided, documentation to be provided, a brief list potentially useful characterization methods that can be leveraged at INL, and other miscellaneous requirements specific to this project. This document is intended for informational use only.

innovative nuclear materials↗

Development and Application of In Situ Nanocharacterization to Photocatalytic Materials for Solar Fuel Generation

Photocatalytic materials offer an attractive approach for converting solar energy into chemical energy but the performance of the current generation of materials is insufficient to make a technology viable. To address this deficiency, it is necessary to develop a fundamental atomic level understanding of the functioning of such materials so that strategies can be developed to improve performance. This project was undertaken to explore the fundamental structure and properties of photocatalytic materials using atomic resolution imaging and spectroscopy techniques available on advanced transmission electron microscopy. Specifically, there is a need to develop an understanding of how atomic structures/defects and nanoparticle configurations regulate electronic, optical, and catalytic properties to facilitate the design of next generation photocatalysts for solar fuel production. The work focused on fundamental materials information that can be gained from advanced transmission electron microscopy study on novel and existing photocatalytic systems with an emphasis on the hydrogen evolution reaction (HER). Throughout the project, new instrumentation and microscopy characterization tools were developed. Two focus areas were: developing in situ TEM methods and advanced electron energy-loss spectroscopic for nanoscale analysis of catalysts. The work spanned a period of 12 years and for convenience, the report is divided into four phases, approximately corresponding to the four funding periods of the program. Most of the significant results are reported in archival journal publications.

36 MATERIALS SCIENCE↗

High-Throughput Characterization Tools/Algorithms To Outline Porosity Variability in AM Samples as a Function of Processing Conditions

This report documents the development and deployment of advanced algorithms and tools that enable high-throughput characterization for metal additive manufacturing (AM), with a particular focus on process parameter optimization and material/part qualification for nuclear applications. While the method ologies presented support diverse characterization techniques, the majority of the work is centered on AI-driven algorithms for X-ray computed tomography (XCT) to accelerate defect detection and materials analysis at scale.

36 MATERIALS SCIENCE↗

Mechanistic Studies Of Combustion And Structure Formation During Combustion Synthesis Of Advanced Materials: Phase Separation Mechanism For Bio-Alloys

Among all implant materials, Co-Cr-Mo alloys demonstrate perhaps the most useful balance of resistance to corrosion, fatigue and wear, along with strength and biocompatibility [1]. Currently, these widely used alloys are produced by conventional furnace technology. Owing to high melting points of the main alloy elements (e.g. Tm.p.(Co) ~1768 K), high-temperature furnaces and long process times (several hours) are required. Therefore, attempts to develop more efficient and flexible methods for production of such alloys with superior properties are of great interest. The synthesis of materials using combustion phenomena is an advanced approach in powder metallurgy [2]. The process is characterized by unique conditions involving extremely fast heating rates (up to 10(exp 6 K/s), high temperatures (up to 3500 K), and short reaction times (on the order of seconds). As a result, combustion synthesis (CS) offers several attractive advantages over conventional metallurgical processing and alloy development technologies. The foremost is that solely the heat of chemical reaction (instead of an external source) supplies the energy for the synthesis. Also, simple equipment, rather than energy-intensive high-temperature furnaces, is sufficient. This work was devoted to experiments on CS of Co-based alloys by utilizing thermite (metal oxide-reducing metal) reactions, where phase separation subsequently produces materials with tailored compositions and properties. Owing to high reaction exothermicity, the CS process results in a significant increase of temperature (up to 3000 C), which is higher than melting points of all products. Since the products differ in density, phase separation may be a gravitydriven process: the heavy (metallic phase) settles while the light (slag) phase floats. The goal was to determine if buoyancy is indeed the major mechanism that controls phase segregation.

Varma, A.↗

Measurement Challenges for Carbon Nanotube Material

The advances in large scale applications of carbon nanotubes demand a reliable supply of raw and processed materials. It is imperative to have a consistent quality control of these nanomaterials to distinguish material inconsistency from the modifications induced by processing of nanotubes for any application. NASA Johnson Space Center realized this need five years back and started a program to standardize the characterization methods. The JSC team conducted two workshops (2003 and 2005) in collaboration with NIST focusing on purity and dispersion measurement issues of carbon nanotubes [1]. In 2004, the NASA-JSC protocol was developed by combining analytical techniques of SEM, TEM, UV-VIS-NIR absorption, Raman, and TGA [2]. This protocol is routinely used by several researchers across the world as a first step in characterizing raw and purified carbon nanotubes. A suggested practice guide consisting of detailed chapters on TGA, Raman, electron microscopy and NIR absorption is in the final stages and is undergoing revisions with input from the nanotube community [3]. The possible addition of other techniques such as XPS, and ICP to the existing protocol will be presented. Recent activities at ANSI and ISO towards implementing these protocols as nanotube characterization standards will be discussed.

Sosa, Edward↗

Characterizing Nanophase Materials on Mars: Spectroscopic Studies of Allophane and Imogolite

Allophane is an amorphous or poorly crystalline hydrous aluminosilicate material. Allophane's chemical structure represents a hollow nanosphere, 5-6 nm in diameter with 4-7 large pores in the structure. Identification of allophane and other amorphous and nanophase minerals on Mars has provided clues about the aqueous geochemical environment there. These materials likely represent partially altered or leached basaltic ash and therefore, could represent a geologic marker for where water was present on the Martian surface; as well as indicate regions of climate change, where surface water was not present long enough or sufficiently warm to form clays. Characterization of these materials is important for increasing spectral recognition capabilities using visible/near-infrared (VNIR) and thermal infrared (TIR) spectra of Mars. A suite of synthetic allophane samples was created using a method that has been modified to produce allophane with Fe isomorphically substituted for Al in octahedral coordination. Compositions of the materials range from high-Si allophane (molar Al:Si = 1:2) to protoimogolite (Al:Si = 2:1), with Fe(3+) and Fe(2+) isomorphically substituted for Al from 0-10 mol% of total Al. These compositions span the range observed in natural terrestrial allophanes. Fe K-edge X-ray absorption spectroscopy provided information on the speciation and electrochemical and structural position of Fe in the framework. Fourier transform infrared spectroscopy confirmed syntheses and demonstrated changes in infrared spectroscopic signature with Fe substitution. VNIR reflectance spectra and TIR Thermal infrared emissivity spectra were also collected for direct comparison to Martian data. By increasing spectral recognition capacities of nanophase materials, more accurate estimates can be made on the aqueous geochemical environment of Mars.

Jeute, Thomas↗

Systems and Methods for Implementing Flexible Members Including Integrated Tools Made from Metallic Glass-Based Materials

Systems and methods in accordance with embodiments of the invention implement flexible members that include integrated tools made from metallic glass-based materials. In one embodiment, a structure includes: a flexible member characterized by an elongated geometry and an integrated tool disposed at one end of the elongated geometry; where the flexible member includes a metallic glass-based material.

Parness, Aaron↗

A guide to transient absorption spectroscopy for porous crystalline materials in photocatalysis

Transient absorption spectroscopy has become an increasingly accessible method for probing the fundamental mechanisms of photocatalytic reaction and has provided important mechanistic insights across a wide range of systems. However, recent studies on metal-organic framework and covalent-organic framework based photocatalysts employ transient absorption primarily as a supplementary characterization technique rather than as a tool for gaining mechanistic insight. This perspective identifies recurring limitations in current practices and outlines strategies for more deliberate application of transient absorption spectroscopy in photocatalysis. By emphasizing clarity in data presentation and interpretation, we aim to elevate transient absorption spectroscopy from a routine characterization tool to a powerful approach for elucidating mechanistic photophysics of framework materials that govern their photocatalytic performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterization of Arsenic and Selenium in Coal Fly Ash to Improve Evaluations for Disposal and Reuse Potential (Final Technical Report)

Coal fly ash is a high volume waste material that is discarded in landfills and surface water impoundments across the U.S. and is also widely recycled for a variety of applications. The leaching of potential of contaminants of concern, such as arsenic (As) and selenium (Se), is often the driver of risk assessments for coal ash disposal and reuse. The extent of leachable As and Se depends on several factors related to environmental conditions and fly ash characteristics. Previous studies employed various methods to delineate the concentration, chemical form, and distribution of As and Se in fly ash materials. However, few studies have attempted to directly correlate these properties to mobilization parameters relevant to disposal and reuse. Instead, the coal residuals industries often rely upon standardized leaching protocols that can be laborious or involve hazardous chemicals. The goals of the project were to: 1) Develop and evaluate a characterization protocol that can be used to screen fly ash samples for leachability of As and Se; 2) Characterize As, Se, and associated constituents of fly ash particles at multiple length scales (nanometer to micrometer) to determine if elemental associations differ as a function of the resolution of characterization; and 3) Establish a predictive model for the chemical composition of coal ash produced annually at major U.S. coal fired power facilities on 50-year national coal supply records. For the first objective, we performed leaching experiments with 52 fly ash samples collected from 15 different U.S. power plants and representing coal feedstocks from the three major domestic coal regions. For this work, we assessed the mobilization potential of As and Se in fly ash based on standardized leaching protocols and performed multivariate and lasso regression analyses to explore correlations of leachable As and Se contents with characteristics such as major element contents, loss on ignition (LOI) and pH. The results of regression models indicated that major elements (Fe, Ca, Al) for a wide range of fly ashes can serve as predictor variables for the leaching potential of As, but not for Se. LOI and pH were not important predictive variables in the models. Both regression approaches resulted in relatively strong fits for leachable As (correlation coefficient R 2 = 0.78 for both models) compared to models for leachable Se (R 2 = 0.49). Overall, these results suggest that correlation models combined with on-site elemental analysis with portable analyzers may enable a screening method for leachable As in coal ash. For the second objective, we utilized nanoscale 2-D imaging (30-50 nm spot size) with the Hard X-ray Nanoprobe (HXN) in combination with microprobe X-ray capabilities (~5 µm resolution) to determine As and Se elemental associations in fly ash particles. Speciation of As and Se was also measured at the nano- to microscale with X-ray absorption spectroscopy. The enhanced resolution of HXN showed As and Se that were diffusely located around or comingled with Ca- and Fe-rich particles. The results also showed nanoparticles of Se attached to the surface of fly ash grains. Overall, a comparison of As and Se species across scales highlights the heterogeneity and complexity of chemical associations for these trace elements of concern in coal fly ash. For the final objective, we developed a predictive model for major element composition of coal ash in reserve at disposal sites of major U.S. coal fired power plants. This model was constructed from coal purchase records of 705 power stations from 1973-2022 and was trained on coal ash composition data showing that coal ash elemental composition is strongly associated with the source of feedstock coal. The model showed regional shifts in the major element contents of ash produced by power plants in the last 50 years, particularly for calcium and iron (expressed as %CaO and %Fe 2 O 3 ), as coal-fired power stations changed their source of coal over this time frame. Our approach enables an estimation of coal ash chemical composition that is stored in waste impoundments at individual power stations. Such information can help delineate the regional market potential for material applications that would utilize coal ash harvested from disposal sites across the U.S.

01 COAL, LIGNITE, AND PEAT↗

Fabrication of High Temperature Cermet Materials for Nuclear Thermal Propulsion

Processing techniques are being developed to fabricate refractory metal and ceramic cermet materials for Nuclear Thermal Propulsion (NTP). Significant advances have been made in the area of high-temperature cermet fuel processing since RoverNERVA. Cermet materials offer several advantages such as retention of fission products and fuels, thermal shock resistance, hydrogen compatibility, high conductivity, and high strength. Recent NASA h d e d research has demonstrated the net shape fabrication of W-Re-HfC and other refractory metal and ceramic components that are similar to UN/W-Re cermet fuels. This effort is focused on basic research and characterization to identify the most promising compositions and processing techniques. A particular emphasis is being placed on low cost processes to fabricate near net shape parts of practical size. Several processing methods including Vacuum Plasma Spray (VPS) and conventional PM processes are being evaluated to fabricate material property samples and components. Surrogate W-Re/ZrN cermet fuel materials are being used to develop processing techniques for both coated and uncoated ceramic particles. After process optimization, depleted uranium-based cermets will be fabricated and tested to evaluate mechanical, thermal, and hot H2 erosion properties. This paper provides details on the current results of the project.

Hickman, Robert↗

Multiplexed Holographic Data Storage in Bacteriorhodopsin

Biochrome photosensitive films in particular Bacteriorhodopsin exhibit features which make these materials an attractive recording medium for optical data storage and processing. Bacteriorhodopsin films find numerous applications in a wide range of optical data processing applications; however the short-term memory characteristics of BR limits their applications for holographic data storage. The life-time of the BR can be extended using cryogenic temperatures [1], although this method makes the system overly complicated and unstable. Longer life-times can be provided in one modification of BR - the "blue" membrane BR [2], however currently available films are characterized by both low diffraction efficiency and difficulties in providing photoreversible recording. In addition, as a dynamic recording material, the BR requires different wavelengths for recording and reconstructing of optical data in order to prevent the information erasure during its readout. This fact also put constraints on a BR-based Optical Memory, due to information loss in holographic memory systems employing the two-lambda technique for reading-writing thick multiplexed holograms.

Mehrl, David J.↗