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At least 73 records · Page 4

Characterization Report for the MP-1 Experiment Fabrication Campaign (Rev.1)

This report covers the results of MP 1 fuel characterization analysis to provide a detailed understanding of the as-fabricated fuel that would be irradiated in the MP 1 (Mini-Plate 1) experiment. The work was performed at Pacific Northwest National Laboratory (PNNL), Idaho National Laboratory (INL), and Los Alamos National Laboratory (LANL). Characterization of the as-fabricated fuel was performed in accordance with Characterization Plan for the Fabrication of U 10Mo for the MP 1 Experiment, hereinafter the MP 1 Characterization Plan (MAQP 2016). Under the MP 1 Characterization Plan, fuel foils at different points in the foil fabrication process (e.g., hot rolled annealed, cold rolled annealed) were studied to understand the effect of various thermomechanical processes on the fuel microstructure. Samples were sent to each of the three organizations so that testing and analysis could be performed independently using similar equipment and a standardized set of measurement and analysis procedures. The MP 1 experiment will provide an opportunity to understand the effects of processing conditions on the final fuel microstructure, to compare independently obtained results, and achieve a three-way validation. PNNL characterized 28 uranium–10 wt% molybdenum (U 10Mo) samples. Six pieces/specimens from each sample/foil were sectioned, in accordance with the MP 1 Characterization Plan. Similarly, INL and LANL also examined 24 and 17 U 10Mo specimens, respectively. These total 69 samples consist of six types of MP 1 characterization foils fabricated by Babcock and Wilcox Technologies (BWXT) from ingots produced by the Y-12 National Security Complex: (a.) 0.047 in.-thick hot-rolled and annealed samples with and without Zr layers; (b.) 0.02 in.-thick cold-rolled and annealed samples with and without Zr layers; and (c.) 0.01 in.-thick cold-rolled and annealed samples with and without Zr layers. Microstructure, chemical composition, carbide morphology, U 10Mo foil thickness, Zr thickness, mechanical properties (microhardness), and density were evaluated in both longitudinal and transverse directions for foils of the three different thicknesses.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Preliminary Results of the Investigation of the Carbonaceous Chondrites Nagoya, Allende, and Murray

As part of a long-term study of morphological biomarkers in Astromaterials, we are documenting a variety of features considered to be indigenous to ancient terrestrial rocks and carbonaceous meteorites. In preparation for the study of samples returned from Mars and other bodies of our Solar System, it is imperative that we establish a database of the nature and morphology of known bacterial fossils in Earth rocks and biomorphic microstructures which may represent microfossils in meteorites. The process of fossilization or mineralization can cause major changes in morphologies and textures of the original organisms and the study of fossilized terrestrial organisms can help provide insight into the interpretation of mineral biomarkers and abiotic microstructures which may mimic certain aspects of microfossils. One class of biomarkers consists of biominerals which have either been precipitated directly by microorganisms, or whose precipitation has been influenced by the organisms. Such microbe-mediated mineral formation may include important clues to the size, shape, and environment of the microorganisms. This paper describes the detection of possible microbe-mediated minerals, biomorphic microstructures and possible microfossils in the Nagoya, Allende, and Murray Carbonaceous Chondrites.

Rozanov, Alexei Yu.↗

Making High-Porosity Alloy Spheroids

Noncontact process yields low-density, porous microstructure. Small spheroids of porous alloys with large surface area per unit volume produced by containerless processing method. Without container walls to serve as nucleation sites, alloy cools to well below normal freezing point without solidifying. Solidification then proceeds rapidly; interdendritic liquid pulled out by growing crystals, resulting in porous microstructure. The more rapid the cooling rate, the faster crystals grow and more porous solid becomes. Drop-tube method useful in creating porous microstructures from other materials including oxides, carbides, and organic materials. Other means of containerless processing - acoustic or air-jet levitation, low-gravity float melting, melt spinning, or jet spraying, adapted to process.

Ethridge, E. C.↗

Investigating Space Weathering of Ryugu Grains Using Electron Microscopy and X-Ray Computed Tomography

The effects of micrometeorite bombardment and solar wind ion irradiation – collectively known as space weathering – alter the microstructural, chemical, and spectral properties of airless surfaces. Characteristics of space weathering include vesiculated textures, amorphous grain rims (upper ~100 nm), and the production of Fe-bearing nanoparticles (npFe). The resulting modifications in the optical properties of the surface regolith include changes in spectral slope and overall reflectance of the surfaces as well as the attenuation of their characteristic absorption bands across VIS-NIR wavelengths. As the surface is continuously exposed to interplanetary space over time, the accrual of these features complicates the interpretation of remote sensing spectral data and the characterization of returned samples. Laboratory experiments that simulate solar wind irradiation and micrometeoroid impacts using carbonaceous analogs have revealed novel and complex microstructural and chemical changes, including the decrease in organic species concentrations and the reduction of Fe 3+ . In 2020, the Japan Aerospace Exploration Agency (JAXA)’s Hayabusa2 mission returned over 5 g of regolith particles from near- Earth C-type asteroid (162173) Ryugu – a unique opportunity to study space weathering on carbonaceous materials. Initial studies have established that the surface morphology and chemical signatures of space weathering in returned samples share characteristics with laser irradiation experiments simulating micrometeoroid bombardment, indicating that impacts are a significant space weathering mechanism operating on Ryugu. Here, we seek to improve our understanding of space weathering of carbonaceous asteroidal regolith grains by characterizing its effects directly on returned samples to determine the nature of space weathering on Ryugu. To do so, we performed coordinated analyses using electron beam techniques and X-ray computed tomography (XCT) to examine the effects of space weathering on grains returned from the surface of Ryugu by the Hayabusa2 mission.

L. E. Melendez↗

Microstructural Evaluation of Phase Instability in Large Bandgap Metal Halide Perovskites

The optoelectronic performance of organic–inorganic halide perovskite (OIHP)-based devices has been improved in recent years. Particularly, solar cells fabricated using mixed-cations and mixed-halides have outperformed their single-cation and single-halide counterparts. Yet, a systematic evaluation of the microstructural behavior of mixed perovskites is missing despite their known composition-dependent photoinstability. Here, we explore microstructural inhomogeneity in (FAPbI 3 ) x (MAPbBr 3 ) 1– x using advanced scanning probe microscopy techniques. In this work, contact potential difference (CPD) maps measured by Kelvin probe force microscopy show an increased fraction of grains exhibiting a low CPD with flat topography as MAPbBr 3 concentration is increased. The higher portion of low CPD contributes to asymmetric CPD distribution curves. Chemical analysis reveals these grains being rich in MA, Pb, and I. The composition-dependent phase segregation upon illumination, reflected on the emergence of a low-energy peak emission in the original photoluminescence spectra, arises from the formation of such grains with flat topology. Bias-dependent piezo-response force microscopy measurements, in these grains, further confirm vigorous ion migration and cause a hysteretic piezo-response. Our results, therefore, provide insights into the microstructural evaluation of phase segregation and ion migration in OIHPs pointing toward process optimization as a mean to further enhance their optoelectronic performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Mechanical Roles of Polysaccharide Assembly and Interactions in Plant Cell Walls

Plants synthesize polysaccharide-based primary cell walls that possess unique microstructures and mechanical properties to accommodate plant growth and provide protection. Here, it remains challenging to assess the role of polysaccharide organization and interactions in the mechanical behavior of primary cell walls owing to their complex microstructure and highly nonlinear mechanical responses. Employing a coarse-grained molecular dynamics model developed for onion epidermal walls, this work explores the conditions under which polysaccharide assembly and interactions might play a significant role in primary cell wall mechanics. Cellulose–cellulose adhesion plays a dominant role in the wall load-bearing capacity, but when cellulose–cellulose adhesion was disrupted computationally, cellulose–xyloglucan adhesion could influence the wall load-bearing capacity. Contrary to the common concept that xyloglucans mechanically tether well-separated cellulose microfibrils, xyloglucans functioned in this case as interfibrillar adhesives capable of transmitting tensile forces between cellulose microfibrils. Our findings may inform design criteria of new materials inspired by plant cell walls.

59 BASIC BIOLOGICAL SCIENCES↗

The hierarchical structure of organic mixed ionic–electronic conductors and its evolution in water

Polymeric organic mixed ionic–electronic conductors underpin several technologies in which their electrochemical properties are desirable. These properties, however, depend on the microstructure that develops in their aqueous operational environment. We investigated the structure of a model organic mixed ionic–electronic conductor across multiple length scales using cryogenic four-dimensional scanning transmission electron microscopy in both its dry and hydrated states. Four-dimensional scanning transmission electron microscopy allows us to identify the prevalent defects in the polymer crystalline regions and to analyse the liquid crystalline nature of the polymer. The orientation maps of the dry and hydrated polymers show that swelling-induced disorder is mostly localized in discrete regions, thereby largely preserving the liquid crystalline order. Therefore, the liquid crystalline mesostructure makes electronic transport robust to electrolyte ingress. Furthermore, this study demonstrates that cryogenic four-dimensional scanning transmission electron microscopy provides multiscale structural insights into complex, hierarchical structures such as polymeric organic mixed ionic–electronic conductors, even in their hydrated operating state.

36 MATERIALS SCIENCE↗

The solidification of monotectic alloys - Microstructures and phase spacings

The microstructures of directionally grown monotectic alloys in metallic and organic systems fall into two categories those which can form aligned fibrous composite structures with even phase spacings and fiber sections, and those in which the phase distribution is coarser and less regular. This division appears to relate to the form of the phase diagram and has been rationalized by Cahn (1977, 1979) in terms of the relative surface energies between solid and two liquids to give steady state or nonsteady state profiles. The transition in growth behavior occurs when the ratio of the monotectic temperature to that of the upper consolute temperature is approximately 0.9. Differences in phase spacings between a range of monotectic and eutectic systems are discussed in terms of the expected growth interface shapes and the factors which will influence them.

Grugel, R. N.↗

Molecular modeling of polymer composite-analyte interactions in electronic nose sensors

We report a molecular modeling study to investigate the polymer-carbon black (CB) composite-analyte interactions in resistive sensors. These sensors comprise the JPL electronic nose (ENose) sensing array developed for monitoring breathing air in human habitats. The polymer in the composite is modeled based on its stereoisomerism and sequence isomerism, while the CB is modeled as uncharged naphthalene rings with no hydrogens. The Dreiding 2.21 force field is used for the polymer, solvent molecules and graphite parameters are assigned to the carbon black atoms. A combination of molecular mechanics (MM) and molecular dynamics (NPT-MD and NVT-MD) techniques are used to obtain the equilibrium composite structure by inserting naphthalene rings in the polymer matrix. Polymers considered for this work include poly(4-vinylphenol), polyethylene oxide, and ethyl cellulose. Analytes studied are representative of both inorganic and organic compounds. The results are analyzed for the composite microstructure by calculating the radial distribution profiles as well as for the sensor response by predicting the interaction energies of the analytes with the composites. c2003 Elsevier Science B.V. All rights reserved.

NASA Center JPL↗

Voltage cycling as a dynamic operation mode for high temperature electrolysis solid oxide cells

Solid Oxide Electrolysis Cells (SOECs) have emerged as a promising technology for the efficient production of H2 via high-temperature electrolysis. However, power input from dynamic energy sources remains a significant challenge for their long-term stability. It is important to analyze the tolerance of cells under dynamic operation conditions. This study focuses on evaluating the impact of voltage cycling on the performance and durability of electrode-supported SOECs. We explore the operational limits and degradation mechanisms of SOECs subjected to various voltage conditions and find that the cells have high tolerance for dynamic voltage. Voltage cycling between 1.3 V and 1.5 V for 9000 cycles does not damage the cell. Conversely, cycling to higher voltages (≥1.7 V) results in accelerated degradation. Advanced characterization is used to screen for various degradation modes post operation. Within the oxygen electrode, XRD and STEM EDS find compositional and phase evolution in all voltage cycled samples including increased decomposition of the air electrode resulting in cation migration. Microstructural analysis of the fuel electrode from nano-CT data shows minimal change throughout the sample set and no evidence of Ni migration, indicating the fuel electrode is stable and not impacted by cycling to higher voltages within the timeframe studied.

Zhu, Zhikuan↗

One thousand soils for molecular understanding of belowground carbon cycling

While significant progress has been made in understanding global carbon (C) cycling, the mechanisms regulating belowground C fluxes and storage are still uncertain. New molecular technologies have the power to elucidate these processes, yet we have no widespread standardized implementation of molecular techniques. To address this gap, we introduce the Molecular Observation Network (MONet), a decadal vision from the Environmental Molecular Sciences Laboratory (EMSL), to develop a national network for understanding the molecular composition, physical structure, and hydraulic and biological properties of soil and water. These data are essential for advancing the next generation of multiscale Earth systems models. In this paper, we discuss the 1000 Soils Pilot for MONet, including a description of standardized sampling materials and protocols and a use case to highlight the utility of molecular-level and microstructural measurements for assessing the impacts of wildfire on soil. While the 1000 Soils Pilot generated a plethora of data, we focus on assessments of soil organic matter (SOM) chemistry via Fourier-transform ion cyclotron resonance-mass spectrometry and microstructural properties via X-ray computed tomography to highlight the effects of recent fire history in forested ecosystems on belowground C cycling. We observed decreases in soil respiration, microbial biomass, and potential enzyme activity in soils with high frequency burns. Additionally, the nominal oxidation state of carbon in SOM increased with burn frequency in surface soils. This results in a quantifiable shift in the molecular signature of SOM and shows that wildfire may result in oxidation of SOM and structural changes to soil pore networks that persist into deeper soils.

54 ENVIRONMENTAL SCIENCES↗

Printing thermoelectric inks toward next-generation energy and thermal devices

The ability of thermoelectric (TE) materials to convert thermal energy to electricity and vice versa highlights them as a promising candidate for sustainable energy applications. Despite considerable increases in the figure of merit zT of thermoelectric materials in the past two decades, there is still a prominent need to develop scalable synthesis and flexible manufacturing processes to convert high-efficiency materials into high-performance devices. Scalable printing techniques provide a versatile solution to not only fabricate both inorganic and organic TE materials with fine control over the compositions and microstructures, but also manufacture thermoelectric devices with optimized geometric and structural designs that lead to improved efficiency and system-level performances. In this review, we aim to provide a comprehensive framework of printing thermoelectric materials and devices by including recent breakthroughs and relevant discussions on TE materials chemistry, ink formulation, flexible or conformable device design, and processing strategies, with an emphasis on additive manufacturing techniques. Additionally, we review recent innovations in the flexible, conformal, and stretchable device architectures and highlight state-of-the-art applications of these TE devices in energy harvesting and thermal management. Perspectives of emerging research opportunities and future directions are also discussed. While this review centers on thermoelectrics, the fundamental ink chemistry and printing processes possess the potential for applications to a broad range of energy, thermal and electronic devices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Electron microscopy data on irradiation effects in glassy carbon, nuclear graphite, pyrolytic carbon, and carbon fibers

Glassy carbon, a monoatomic allotrope of carbon, is a candidate material for components in fission nuclear power systems due to its radiation tolerance. This article presents comprehensive electron microscopy data revealing the effects of neutron and electron irradiation on glassy carbon. For comparison, additional data are provided for pyrolytic graphite and carbon fibers, materials that exhibit similar structural behavior under irradiation. In situ electron irradiation experiments further illustrate the real-time microstructural evolution of glassy carbon during exposure. The dataset is organized into five parts: (1) transmission electron microscopy (TEM) micrographs of as-received and neutron-irradiated glassy carbon; (2) TEM micrographs of neutron-irradiated graphite; (3) TEM micrographs of unirradiated and irradiated carbon–carbon composites; (4) TEM micrographs of pyrolytic carbon specimens in both conditions; (5) scanning transmission electron microscopy (STEM) micrographs of as-received and neutron-irradiated glassy carbon and (6) in situ electron irradiation data of a glassy carbon particle. These datasets provide valuable insights into radiation-induced structural changes in carbon-based materials relevant to nuclear applications.

36 MATERIALS SCIENCE↗

Robust dynamic operation of high temperature electrolysis solid oxide cells

Here, this study evaluates the durability of Ni/YSZ-supported SOECs under dynamic operating conditions relevant to real-world applications. Systematic tests were conducted to assess cell performance under steam cycling (3 to 75% humidified H 2 ), mode cycling between SOFC and SOEC operation, thermal cycling (150 to 750 °C at OCV, and 600 to 800 °C at 1.3V), and redox cycling (between 50% humidified H 2 and 50% humidified N 2 ). Steam cycling, mode cycling, and thermal cycling at OCV do not significantly accelerate performance degradation. Thermal cycling at 1.3V caused minimal damage within 600 to 800 °C. Full redox cycling (multi-hour oxidation holds) induced cell structural failure, while partial redox cycling (0.5 h holds) was tolerated. Extensive characterization revealed some material evolution, namely Sr and Co secondary phase formation, within the oxygen electrode due to La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-δ instability, especially for steam cycling and mode cycling. Minimal changes were identified within the Ni-YSZ fuel electrodes. These findings provide critical insights into SOEC reliability under dynamic conditions, supporting their application in dynamic or intermittent energy systems.

08 HYDROGEN↗

Modeling deformation and failure in AlSi-polyester abradable sealcoating material using microstructure-based finite element simulation

A plasma-sprayed aluminum-silicon (AlSi)/polyester coating is applied in modern gas turbine engines as an abradable sealcoating to maintain tight clearances between the rotating blades and the static casing. While running the engine, the rotating blades “rub” with the abradable coating, which results in extreme strain rate (up to 10 6 ) dynamics and a high-temperature environment. Due to the difficulty of collecting direct measurements, predictive computational models are important for analyzing the deformation and failure of the abradable material, to help meet the design target of avoiding damage to the blade tip and maintaining high fuel efficiency. In this research, a microstructure-based finite element (FE) computational model was developed to capture the complex mechanical behavior of the AlSi/polyester microstructure. The model is based on a virtual representative-volume-element (RVE) of a metal-polymer microstructure, reconstructed from x-ray computed tomography. It models the plastic deformation of, and damage to, each AlSi and polyester constituents, as well as the failure at their interface. The model was calibrated and validated with uniaxial tension and compression experiments, conducted at two temperatures (298 K and 533 K) at an applied strain rate of 10 3 - 10 4 s -1 . The material exhibited strongly asymmetric tension-compression behavior and a sensitivity to temperature, which was well captured by the model. The model was further applied to investigate changes in mechanical behavior due to variations in constituents’ volume fractions, which provides guidance to the microstructural design of AlSi/polyester abradable materials. The model is expected to facilitate the development of improved abradable materials by bypassing the conventional trial-and-error approach and extensive testing requirements.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Kinetics of Pyrolysis and Thermal Evolution of Negev Desert Lithologies

The Negev desert in Israel is home to large quantities of organic-rich, shallow marine sedimentary lithologies that could potentially accommodate the disposal of spent nuclear fuel. Previous thermal analyses of Negev carbonates have focused on industrially relevant considerations such as natural gas and oil extraction or pyrolysis for recovering hydrocarbon fuels. Here, this study addresses thermal evolution of the Negev organic-rich carbonate, siliceous, and phosphorite rocks and associated chemical, mineralogical, and microstructural changes that may occur under prolonged thermal loading in the vicinity of spent nuclear fuel disposal systems. Our employed methods include high-temperature X-ray diffraction, high-temperature infrared spectroscopy, and thermal analysis integrating thermogravimetry, differential scanning calorimetry, and mass spectrometry. Further, we apply iterative iso-conversional model-free methods to derive kinetic parameters for thermal decomposition of the Negev organic-rich carbonate rocks from 200 to 550 °C. Our results have provided mechanistic insights into the thermal evolution encompassing water desorption, decomposition of organic matter, and decarbonation of carbonate phases.

58 GEOSCIENCES↗

Microstructured ion-conducting composites and uses thereof

A composite membrane with nanostructured inorganic and organic phases is applied as an ion-selective layer to prove processability, prevent dendrite shorting, and increase power output of lithium-metal anodes through better Li-ion conductivity. Nanoconfinement, as opposed to macroscale confinement, is known to dramatically alter the properties of bulk materials. Control over a ceramic's size, shape, and properties is achieved with polymer templates. This is a new composition of matter and unique approach to composite membrane design.

Frischmann, Peter David↗

Mapping Structure and Rheology of pH-Responsive Resins for Low-VOC Coatings

In recent years, the paint and coatings industry has shifted away from traditional resin formulations that require high concentrations of volatile organic compounds (VOCs) to achieve the desired rheological performance and sustainability targets. One approach to eliminate or reduce VOCs in paint and coating formulations while maintaining the final performance is to disperse stimuli-responsive polymer latex particles in water. The chemistry and architecture of these particles have been engineered such that the suspension rheology changes in response to the pH changes. The particles can also be swollen with organic solvents to illicit similar rheological changes. To understand how the particle microstructure influences the observed macroscopic properties, we use small-angle neutron scattering and dynamic light scattering to determine that these particles consist of a cross-linked core with long polymer tails that extend into the dispersing medium. Carboxylic acid groups present on the tails deprotonate with increasing pH, and the extension of the polymer chain due to charge repulsion increases the hydrodynamic drag on the particle. Here we find that adjusting the pH alone has a much more significant effect on the shear dependence of the viscosity of the studied resin than adding organic solvent alone. We also find that this resin architecture is more responsive per mole of pH-responsive group than other architectures of pH-responsive latex particles in the literature.

36 MATERIALS SCIENCE↗