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At least 775 records · Page 43

Goals and Progress for Mil Handbook 17, Vol. 5 on Ceramic Matrix Composites: Testing and Characterization

The initial edition of the Mil Handbook 17, Vol. 5 on ceramic matrix composites (CMCs) was recently published. Part C of this CMC volume describes procedures for characterization of the thermal, physical, and mechanical properties of CMCs and subsequent data analysis procedures. As is the case for entire CMC volume, this chapter is a "work in progress" with sections on recommended test plans and matrices, data reduction, and test methods. This presentation will describe the current status in development of this section of the CMC volume and will highlight examples of critical issues that will be addressed in this volume. CMC systems are a different class of material than metals or polymer matrix composite with different mechanical response and failure modes, design rules, test methods, and characterization techniques. The CMC test protocols need to include guidance on how to generate enough reliable data in order to estimate, with reasonable confidence, the lower bounds of performance properties, such as strength and life. Strength data sets on two material systems, C/SiC and Nicalon/SiNC, and a creep rupture data set on C/SiC, will be presented to highlight this issue. The structural properties of CMC parts can sometimes be significantly different than those obtained from flat panels because of changes in fiber architecture often required to make shapes and spatial and lot-to-lot variations in processing conditions. To illustrate an example, the hoop tensile properties of SiC/SiC cylinders will be compared to properties obtained from flat panels fabricated from the same composites. These CMC testing-design issues are being defined and documented in the Mil Handbook 17 CMC volume.

Verrilli, Michael J.↗

Characterization of Dendritic Spatially Extended 3D Patterns in Directional Solidification: Microgravity Experiments in DECLIC-DSI onboard ISS and 3D Phase-field Simulations

To clarify and characterize the fundamental physical mechanisms active in the dynamical formation of three-dimensional (3D) arrays of dendrites under diffusive growth conditions, in situ monitoring of series of experiments on transparent model alloy succinonitrile – 0.46 wt% camphor was carried out under low gravity in the DECLIC Directional Solidification Insert onboard the International Space Station. These experiments offer the very unique opportunity to observe in situ and characterize the dynamics of the microstructure formation and evolution in extended 3D patterns under microgravity environment. The analyses of the dendritic patterns for a broad range of growth velocities displaying different levels of sidebranching will be presented. Especially, the time evolution of primary spacing, in case of solidifications at constant pulling rate as well as for experiments with pulling rate jump, will be compared to 3D phase-field simulations, and the results will be discussed in terms of stable spacing range.

Kaihua Ji↗

Characterization of Dendritic Spatially Extended 3D Patterns in Directional Solidification: Microgravity Experiments in DECLIC-DSI Onboard ISS and 3D Phase-field Simulations

To clarify and characterize the fundamental physical mechanisms active in the dynamical formation of three-dimensional (3D) arrays of dendrites under diffusive growth conditions, in situ monitoring of series of experiments on transparent model alloy succinonitrile – 0.46 wt% camphor was carried out under low gravity in the DECLIC Directional Solidification Insert onboard the International Space Station. These experiments offer the very unique opportunity to observe in situ and characterize the dynamics of the microstructure formation and evolution in extended 3D patterns under microgravity environment. The analyses of the dendritic patterns for a broad range of growth velocities displaying different levels of sidebranching will be presented. Especially, the time evolution of primary spacing, in case of solidifications at constant pulling rate as well as for experiments with pulling rate jump, will be compared to 3D phase-field simulations, and the results will be discussed in terms of stable spacing range.

Kaihua Ji↗

Activation and surface reactions of CO and H 2 on ZnO powders and nanoplates under CO hydrogenation reaction conditions

Here, activation and surface reactions of CO and H 2 on ZnO powders and nanoplates under CO hydrogenation reaction conditions were (quasi) in situ studied using temperature programmed surface reaction spectra, diffuse reflectance Fourier transform infrared spectroscopy, inelastic neutron scattering spectroscopy and electron paramagnetic resonance. CO undergoes disproportion reaction to produce gaseous CO 2 and surface carbon adatoms, and adsorbs to form surface formate species. H 2 adsorption forms dominant irreversibly-adsorbed surface hydroxyl groups and interstitial H species and very minor surface Zn-H species. Surface formate species and hydroxyl groups react to produce CO 2 and H 2 , while surface carbon adatoms are hydrogenated by surface Zn-H species sequentially to produce CH(a), CH 2 (a), CH 3 (a) and eventually gaseous CH 4 . The ZnO nanoplates, exposing a higher fraction of Zn-ZnO(0001) and O-ZnO(000–1) polar facets, are more active than the ZnO powders to catalyze CO hydrogenation to CH 4 . These results provide fundamental understanding of the reaction mechanisms and structural effects of CO hydrogenation reaction catalyzed by ZnO-based catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Baseline Graphite Characterization

Baseline Graphite Characterization: Purpose of Baseline, Mechanical Baseline Tests, Physical Properties Tests, Methodology, Baseline progress, Density, Ultimate Tensile Strength, PCEA Ultimate Tensile Strength, Split Disc Tests, Compression Tests, Flexural Tests, and Coefficient of Thermal Expansion.

22 - GENERAL STUDIES OF NUCLEAR REACTORS↗

Resolving Nanoscale Processes during Carbon Mineralization Using Identical Location Transmission Electron Microscopy

Basalt reservoirs offer the potential for carbon mineralization, aiding in achieving net-zero emissions. However, debates persist about microscopic crystallization mechanisms due to limited characterization techniques under high-temperature and pressure conditions. By using Identical Location Transmission Electron Microscopy (IL-TEM) and cryo-TEM, this study reveals nanoscale interfacial carbonation processes of forsterite and diopside nanoparticles in water-saturated supercritical carbon dioxide under realistic reservoir conditions. Further, both minerals undergo preferential metal cation dissolution into a thin water film, forming porous Si-rich amorphous layers, supporting the leached layer mechanism as the dominant mineral reactivity process. Diopside’s amorphous layer has lower porosity and growth rate relative to forsterite, likely related to the connectivity of silicate tetrahedra. Kinetically favorable nesquehonite and aragonite nanocrystals form on the amorphous layers. These findings support the development of accurate reservoir simulations and help enable commercial-scale carbon storage deployment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterize traction–separation relation and interfacial imperfections by data-driven machine learning models

Abstract Interfacial mechanical properties are important in composite materials and their applications, including vehicle structures, soft robotics, and aerospace. Determination of traction–separation (T–S) relations at interfaces in composites can lead to evaluations of structural reliability, mechanical robustness, and failures criteria. Accurate measurements on T–S relations remain challenging, since the interface interaction generally happens at microscale. With the emergence of machine learning (ML), data-driven model becomes an efficient method to predict the interfacial behaviors of composite materials and establish their mechanical models. Here, we combine ML, finite element analysis (FEA), and empirical experiments to develop data-driven models that characterize interfacial mechanical properties precisely. Specifically, eXtreme Gradient Boosting (XGBoost) multi-output regressions and classifier models are harnessed to investigate T–S relations and identify the imperfection locations at interface, respectively. The ML models are trained by macroscale force–displacement curves, which can be obtained from FEA and standard mechanical tests. The results show accurate predictions of T–S relations ( R 2 = 0.988) and identification of imperfection locations with 81% accuracy. Our models are experimentally validated by 3D printed double cantilever beam specimens from different materials. Furthermore, we provide a code package containing trained ML models, allowing other researchers to establish T–S relations for different material interfaces.

97 MATHEMATICS AND COMPUTING↗

Advanced Characterization of Thin Film Solar Cells

Polycrystalline thin-film solar cells have reached a levelized cost of energy that is competitive with all other sources of electricity. The technology has significantly improved in recent years, with laboratory cell efficiencies for cadmium telluride (CdTe), perovskites, and copper indium gallium diselenide (CIGS) each exceeding 22 percent. Both CdTe and CIGS solar panels are now produced at the gigawatt scale. However, there are ongoing challenges, including the continued need to improve performance and stability while reducing cost. Advancing polycrystalline solar cell technology demands an in-depth understanding of efficiency, scaling, and degradation mechanisms, which requires sophisticated characterization methods. These methods will enable reseachers and manufacturers to improve future solar modules and systems. This work provides researchers with a concise overview of the status of thin-film solar cell technology and characterization. Chapters describe material systems and their properties and then provide an in-depth look at relevant characterization methods and the learning facilitated by each of these. Following an introductory chapter, the book provides systematic and thorough coverage of the following topics: trends to improve CdTe solar cell performance; Cu(In,Ga)Se2 and related materials; perovskite solar cells; photovoltaic device modelling; luminescence and thermal imaging of thin-film photovoltaic materials, devices, and modules; application of spatially resolved spectroscopy characterization techniques on Cu2ZnSnSe4 solar cells; time-resolved photoluminescence characterization of polycrystalline thin-film solar cells; fundamentals of electrical material and device spectroscopies applied to thin-film polycrystalline chalcogenide solar cells; nanometer-scale characterization of thin-film solar cells by atomic force microscopy-based electrical probes; scanning transmission electron microscopy characterization of solar cells; photoelectron spectroscopy methods in solar cell research; time-of-flight secondary-ion mass spectrometry and atom probe tomography; and solid-state nuclear magnetic resonance characterization for photovoltaic applications. The final chapter provides an overview and describes future prospects.

41 EE - Solar Energy Technologies Office (EE-4S)↗

Characterization of ionic currents of cells of the subfornical organ that project to the supraoptic nuclei

The subfornical organ (SFO) is a forebrain structure that converts peripheral blood-borne signals reflecting the hydrational state of the body to neural signals and then through efferent fibers conveys this information to several central nervous system structures. One of the forebrain areas receiving input from the SFO is the supraoptic nucleus (SON), a source of vasopressin synthesis and control of release from the posterior pituitary. Little is known of the transduction and transmission processes by which this conversion of systemic information to brain input occurs. As a step in elucidating these mechanisms, the present study characterized the ionic currents of dissociated cells of the SFO that were identified as neurons that send efferents to the SON. A retrograde tracer was injected into the SON area in eleven-day-old rats. After three days for retrograde transport of the label, the SFOs of these animals were dissociated and plated for tissue culture. The retrograde tracer was used to identify the soma of SFO cells projecting to the SON so that voltage-dependent ionic currents using whole-cell voltage clamp methods could be studied. The three types of currents in labeled SFO neurons were characterized as a 1) rapid, transient inward current that can be blocked by tetrodotoxin (TTX) characteristic of a sodium current; 2) slow-onset sustained outward current that can be blocked by tetraethylammonium (TEA) characteristic of a delayed rectifier potassium current; and 3) remaining outward current that has a rapid-onset and transient characteristic of a potassium A-type current. Copyright 1999 Elsevier Science B.V.

Non-NASA Center↗

Characterization of Large Batch 14YWT Heat (NFA-2) for JOYO Irradiations (Rev.1)

The development and deployment of advanced cladding materials in advanced reactors requires the collection of relevant performance data for each cladding concept. Novel cladding concepts typically undergo significant innovation and iteration over the course of their development, and intention should be given to providing a snapshot of present performance. Thus, a modern heat of the nanostructured ferritic alloy (NFA) 14YWT is produced using state-of-the-art procedures for impurity minimization combined with thermomechanical processing methods designed to optimize fracture toughness, tensile strength, and ductility. This new heat of 14YWT, NFA-2, will provide the Advanced Fuels Campaign with adequate material for upcoming irradiation and mechanical testing campaigns. This report outlines procurement of new gas atomized 14YWT powder, production of four new bars of 14YWT, and subsequent mechanical and microstructural property characterization.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

A General Closed-Form Solution for the Lunar Reconnaissance Orbiter (LRO) Antenna Pointing System

The National Aeronautics and Space Administration s (NASA) Lunar Reconnaissance Orbiter (LRO) launched on June 18, 2009 from the Cape Canaveral Air Force Station aboard an Atlas V launch vehicle into a direct insertion trajectory to the Moon LRO, designed, built, and operated by the NASA Goddard Space Flight Center in Greenbelt, MD, is gathering crucial data on the lunar environment that will help astronauts prepare for long-duration lunar expeditions. During the mission s nominal life of one year its six instruments and one technology demonstrator will find safe landing site, locate potential resources, characterize the radiation environment and test new technology. To date, LRO has been operating well within the bounds of its requirements and has been collecting excellent science data images taken from the LRO Camera Narrow Angle Camera (LROC NAC) of the Apollo landing sites have appeared on cable news networks. A significant amount of information on LRO s science instruments is provided at the LRO mission webpage. LRO s Attitude Control System (ACS), in addition to controlling the orientation of the spacecraft is also responsible for pointing the High Gain Antenna (HGA). A dual-axis (or double-gimbaled) antenna, deployed on a meter-long boom, is required to point at a selected Earth ground station. Due to signal loss over the distance from the Moon to Earth, pointing precision for the antenna system is very tight. Since the HGA has to be deployed in spaceflight, its exact geometry relative to the spacecraft body is uncertain. In addition, thermal distortions and mechanical errors/tolerances must be characterized and removed to realize the greatest gain from the antenna system. These reasons necessitate the need for an in-flight calibration. Once in orbit around the moon, a series of attitude maneuvers was conducted to provide data needed to determine optimal parameters to load onboard, which would account for the environmental and mechanical errors at any antenna orientation. The nominal geometry for the HGA involves an outer gimbal axis that is exactly perpendicular to the inner gimbal axis, and a target direction that is exactly perpendicular to the outer gimbal axis. For this nominal geometry, closed-form solutions of the desired gimbal angles are simple to get for a desired target direction specified in the spacecraft body fame. If the gimbal axes and the antenna boresight are slightly misaligned, the nominal closed-form solution is not sufficiently accurate for computing the gimbal angles needed to point at a target. In this situation, either a general closed-form solution has to be developed for a mechanism with general geometries, or a correction scheme has to be applied to the nominal closed-form solutions. The latter has been adopted for Solar Dynamics Observatory (SDO) as can be seen in Reference 1, and the former has been used for LRO. The advantage of the general closed-form solution is the use of a small number of parameters for the correction of nominal solutions, especially in the regions near singularities. Singularities here refer to cases when the nominal closed-form solutions have two or more solutions. Algorithm complexity, however, is the disadvantage of the general closed-form solution.

Shah, Neerav↗

Micropillar Compression of Additively Manufactured 316L Stainless Steels after 2 MeV Proton Irradiation: A Comparison Study between Planar and Cross-Sectional Micropillars

A micropillar compression study with two different techniques was performed on proton-irradiated additively manufactured (AM) 316L stainless steels. The sample was irradiated at 360 °C using 2 MeV protons to 1.8 average displacement per atom (dpa) in the near-surface region. A comparison study with mechanical test and microstructure characterization was made between planar and cross-sectional pillars prepared from the irradiated surface. While a 2 MeV proton irradiation creates a relatively flat damage zone up to 12 µm, the dpa gradient by a factor of 2 leads to significant dpa uncertainty along the pillar height direction for the conventional planar technique. Cross-sectional pillars can significantly reduce such dpa uncertainty. From one single sample, three cross-sectional pillars were able to show dpa-dependent hardening. Furthermore, post-compression transmission electron microscopy allows the determination of the deformation mechanism of individual micropillars. Cross-sectional micropillar compression can be used to study radiation-induced mechanical property changes with better resolution and less data fluctuation.

transmission electron microscopy↗

Build orientation, surface roughness, and scan path influence on the microstructure, mechanical properties, and flexural fatigue behavior of Ti–6Al–4V fabricated by electron beam melting

In the present work, microstructure and fatigue behavior of Electron Beam Melted (EBM) Ti–6Al–4V have been systematically studied. Fatigue behavior was investigated using four-point bend tests of rectangular bars with internal features fabricated with different build orientations, scan paths, and surface conditions. Microstructural variations were evaluated by optical microscopy and Vickers micro-hardness indentations, both of which were found to be consistent throughout the build and within ranges reported in the literature. The fatigue performance of the EBM material was comparable to wrought Ti–6Al–4V when the loading direction was parallel to the build direction, but severely limited when loaded perpendicular to the build direction or if surface roughness defects were present. Scanning electron microscopy and interrupted fatigue tests were utilized to characterize fracture surfaces, failure mechanisms, crack initiation, and propagation behavior. Crack initiation sites in the vertically-oriented specimens were identified to be melt-related defects formed by insufficient melting.

36 MATERIALS SCIENCE↗

Establishment of a Vertically Integrated Domestic Manufacturing Process for Production of Substrates Needed for Manufacture of Gas Diffusion Layers

In this project, AvCarb, LLC evaluated the baseline performance metrics of commercial carbon veils and their corresponding Gas Diffusion Layers (GDLs) with the goal of establishing an optimized, vertically integrated production system for wet-laid nonwoven substrates used in gas diffusion media for electrochemical energy storage and conversion devices. Mechanical testing and microstructural characterization were conducted and used to develop a multiscale computational model capable of simulating and predicting the performance of GDLs in fuel cells. Although the project successfully generated foundational transport and modeling data, it was terminated prior to identifying the critical GDL design parameters necessary for full optimization. The program aimed to improve carbon veil fabrication through enhanced fiber dispersion, fiber-fiber adhesion control, and improved web formation, enabling the production of high-quality, uniform substrates. Simulations were intended to guide mixing and solution delivery system design and process conditions, followed by production-scale trials to evaluate fiber dispersion, web uniformity, and mechanical robustness. At full deployment, the proposed production line would have been capable of producing approximately 650,000 m² of carbon veil annually. This capability remains strategically important, as the United States currently lacks a domestic source of wet-laid nonwoven carbon substrates that satisfy the stringent quality requirements for fuel-cell GDLs and electrolyzers representing an ongoing supply-chain vulnerability. Beyond supply-chain benefits, the project established a robust benchmarking dataset for existing commercial carbon veils while advancing next-generation material concepts targeting improved performance and manufacturing consistency.

Olson, Cynthia Lemay↗

Temperature- and Rate-Dependent Pathways in Formation of Metastable Silicon Phases under Rapid Decompression

High-pressure metallic beta-Sn silicon (Si-II), depending on temperature, decompression rate, stress, etc., may transform to diverse metastable forms with promising semiconducting properties under decompression. However, the underlying mechanisms governing the different transformation paths are not well understood. Here, two distinctive pathways, viz., a thermally activated crystal-crystal transition and a mechanically driven amorphization, were characterized under rapid decompression of Si-II at various temperatures using in situ time-resolved x-ray diffraction. Under slow decompression, Si-II transforms to a crystalline bc8/r8 phase in the pressure range of 4.3-9.2 GPa through a thermally activated process where the overdepressurization and the onset transition strain are strongly dependent on decompression rate and temperature. In comparison, Si-II collapses structurally to an amorphous form at around 4.3 GPa when the volume expansion approaches a critical strain via rapid decompression beyond a threshold rate. The occurrence of the critical strain indicates a limit of the structural metastability of Si-II, which separates the thermally activated and mechanically driven transition processes. The results show the coupled effect of decompression rate, activation barrier, and thermal energy on the adopted transformation paths, providing atomistic insight into the competition between equilibrium and nonequilibrium pathways and the resulting metastable phases.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Non -degenerate marginal-likelihood calibration with application to quantum characterization

Here, we propose a marginal likelihood strategy within the Kennedy-O’Hagan (KOH) Bayesian framework, where a Gaussian process (GP) models the discrepancy between a physical system and its simulator. Our approach introduces a novel marginalized likelihood by integrating out the degenerate eigenspace of the covariance matrix, rather than approximating the original likelihood. Unlike approximation methods that compromise accuracy for computational efficiency, our method defines an exact likelihood—distinct from the original but preserving all relevant information. This formulation achieves computational efficiency and stability, even for large datasets where the covariance matrix nears degeneracy. Applied to the characterization of a superconducting quantum device at Lawrence Livermore National Laboratory, the approach enhances the predictive accuracy of the Lindblad master equations for modeling Ramsey measurement data by effectively quantifying uncertainties consistent with the quantum data.

general physics↗

Probing the Mechanical Performance of Micro-architected Porous Structures Through In Situ Characterization and Analysis

Micropores play critical roles in both natural and man-made materials. Such pores take on a variety of shapes and sizes ranging from spherical to irregular sphere-like voids with diameters spanning from the nanometer to millimeter scales. When porous structures are mechanically loaded, the pores direct the stress around their free surfaces, altering the material’s mechanical response relative to fully dense materials. In this study, for the first time, we create micro-architected porous samples using nanolithography and investigate the role of pore morphology by conducting a series of in situ micropillar compression tests in scanning electron microscopy. The findings demonstrate that porosity is the primary factor influencing the mechanical response of these micro-architected materials, as often seen on a macroscopic level. Additionally, we observed that pore geometry had a significant impact on Young’s modulus, yield stress, and strain energy density as a secondary parameter. Then, the extracted Young’s modulus was compared to macroscopic empirical models and determined the analytical models sufficiently described the impact of porosity in the microscopic scale but failed to capture the impact of second-order parameters. Furthermore, these results suggest how porous materials can be tailored to achieve desired mechanical properties based on the engineering applications of interest.

36 MATERIALS SCIENCE↗

Separate-Effects Tests for Studying Temperature-Gradient-Driven Cracking in UO 2 Pellets

We report a variety of normal operation and accident scenarios can generate thermal stresses large enough to cause cracking in light-water reactor (LWR) fuel pellets. Cracking of fuel pellets can lead to reduced heat removal, higher centerline temperatures, and localized stress in cladding, all of which impact fuel performance. It is important to experimentally characterize the thermal and mechanical behavior in the pellet before and after cracking to improve cracking models in fuel performance codes. However, in-reactor observation and measurement of cracking is very challenging due to the harsh environment and logistics. Recently, an experimental pellet cracking test stand was developed for separate effects testing of normal operations and accident temperature conditions, using thermal imaging to capture the pellet surface temperature for evaluation of thermal stresses and optical imaging to capture the evolution of cracking in real time. Experiments were performed using depleted uranium dioxide (UO 2 ) pellets, which are useful for collecting data valuable for development and validation of cracking models. A combination of induction and resistance heating was used to create an average temperature gradient of 236°C/cm and 193°C/cm before and after cracking respectively. Characterization of the pellets were done before as well as after cracking. The cracking patterns are somewhat different than those expected in a typical reactor because of the differences in thermal conditions and pellet microstructure. However, if the actual conditions of these experiments are reproduced in computational models, these out-of-pile tests on UO 2 pellets provide relevant data for modeling purposes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗