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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Materials Characterization, Prediction, and Control Project: Characterization of 316L Stainless Steel after Solid Phase Processing using Ultrasonic NDE Method

The Pacific Northwest National Laboratory undertook the Materials Characterization, Prediction, and Control Laboratory Directed Research and Development Project to advance understanding of nuclear material processing and enable multifold acceleration in the development and qualification of new material systems produced via advanced manufacturing methods, such as solid phase processing, for use in national security and advanced energy applications (Smith 2021). A motivation of the Materials Characterization, Prediction, and Control Project was to demonstrate ultrasonic testing as a nondestructive evaluation method to complement traditional destructive methods for characterizing material microstructure with emphasis on grain size determination using a method that may have future applications for real-time inline process monitoring. The objective of the work described in this report is to establish the process and an analysis method for measuring grain sizes of polycrystalline metals with ultrafine grains using ultrasonic shear wave backscattering, building on prior studies on coarser-grained material. The work involves five tasks: Measured ultrasonic backscattering experimentally for a series of 316L stainless steel specimens with various grain sizes made by friction stir processing. Calculated ultrasonic backscattering coefficients from experimental data based on a physical measurement model. Measured ground truth grain sizes of the specimens from electron backscatter diffraction grain boundary images using a generalization of the ASTM E112 (ASTM 2021) intercept method. Built a curve of ultrasonic backscattering coefficients versus the ground truth intercept-based grain sizes to determine the correlation between mean grain sizes and ultrasonic measurements. Demonstrated the ability of using the correlation curve to deduce grain sizes with measured ultrasonic backscattering coefficients for a few 316L stainless steel specimens whose grain sizes were unknown beforehand but were targeted to be an extrapolation to larger grain sizes than used to formulate the correlation curves. Experimental procedures and computational algorithms are developed and validated for these tasks. This work establishes an ultrasonic technique for characterizing material microstructure with ultrafine grains that are often resulted by solid-phase processing. The technique is nondestructive, and it has the potential to be used for real time inline process monitoring. This work successfully demonstrates the viability of an ultrasonic nondestructive evaluation method for microstructural characterization of material having ultrafine grain structure (as small as 1?mm) and produced by an advanced manufacturing method. This includes a demonstration of the method to extrapolate to other conditions. While not demonstrated here, the method is expected to be viable for in-line, or near-inline, process monitoring in advanced manufacturing applications with suitable consideration for access of instrumentation to the material being manufactured.

316 L Stainless Steel↗
DOE OSTI2025

Examples of X-Ray Characterization Techniques in Energy Storage Research

Lithium-ion batteries have revolutionized the portable electronics and transportation sectors. Their performance is often critically dependent on the crystal structures of the anode and cathode electrode materials, which must enable the transport and reversible storage of lithium ions into and out of the lattice. Because lithium is a low-Z element, characterization of materials for lithium-ion batteries can be particularly challenging. Regardless, X-ray techniques enable analysis of material structures to better understand how battery materials perform and degrade, particularly when combined with other materials characterization and electrochemical characterization techniques. While X-ray techniques are most often used in battery research for phase identification of crystal structures, X-ray characterization techniques are also used for a wide variety of other purposes. I will discuss several examples from my research with various collaborators on several projects that highlight the impact that X-ray characterization techniques can have on battery research. The first example will focus on low-temperature microwave-assisted solvothermal synthesis of vanadium-doped LiFePO4 cathode materials for lithium-ion batteries. (1,2) Through a combination of electrochemical and materials characterization, we determined that low temperature synthesis resulted in metastable phases that enabled incorporation of higher dopant levels than resulting from high-temperature synthesis of thermodynamically stable phases. Rietveld refinement of X-ray diffraction data enabled understanding of how lattice parameters changed with doping levels and synthesis temperature. X-ray absorption near edge spectroscopy enabled understanding of the vanadium and iron oxidation states to confirm how vacancies in the structure caused by doping were charge compensated. This was important to understand because the literature suggests doping can improve LiFePO4 electrical conductivity, which improves battery charge and discharge rates. The second example will focus on understanding residual strain in lithium metal anodes. Lithium-ion batteries typically use graphite anodes, but the charge-storage capacity can be theoretically improved ~10x by using lithium metal as the anode material instead. However, lithium anodes suffer from growth of high-aspect-ratio features, such as dendrites, that can pierce nanoporous polymer separators and lead to short circuits and fires. External pressure is commonly applied to cells to enable better morphological control. We hypothesized that applied pressure may promote strain and possibly work hardening during electrochemical cycling, which motivated us to look for evidence of residual strain in lithium metal cycled under applied pressure using X-ray diffraction and sin2(..psi..) analysis. We found that lithium electrodeposited under high pressure exhibited in-plane compressive strain and that that lithium electrodeposited under low pressure did not. (3) The residual strain that accompanies electrodeposition under high pressure may lead to work hardening, which may explain how a soft metal like lithium can puncture separators and why higher pressure does not always decrease short circuits. (4-6) References: 1) Harrison, K. L.; Manthiram, A. Microwave-Assisted Solvothermal Synthesis and Characterization of Metastable LiFe1- x (VO) x PO4 Cathodes. Inorganic chemistry 2011, 50(8), 3613-3620. 2) Harrison, K. L.; Bridges, C. A.; Paranthaman, M. P.; Segre, C. U.; Katsoudas, J.; Maroni, V. A.; Idrobo, J. C.; Goodenough, J. B.; Manthiram, A. Temperature Dependence of Aliovalent-Vanadium Doping in LiFePO4 Cathodes. Chemistry of Materials 2013, 25(5), 768-781. 3) Rodriguez, M. A.; Harrison, K. L.; Goriparti, S.; Griego, J. J.; Boyce, B. L.; Perdue, B. R. Use of a Be-Dome Holder for Texture and Strain Characterization of Li Metal Thin Films via Sin2 (..psi..) Methodology. Powder Diffraction 2020, 35(2), 89-97. 4) Jungjohann, K. L.; Gannon, R. N.; Goriparti, S.; Randolph, S. J.; Merrill, L. C.; Johnson, D. C.; Zavadil, K. R.; Harris, S. J.; Harrison, K. L. Cryogenic Laser Ablation Reveals Short-Circuit Mechanism in Lithium Metal Batteries. ACS Energy Letters 2021, 6(6), 2138-2144. 5) Harrison, K. L.; Merrill, L. C.; Long, D. M.; Randolph, S. J.; Goriparti, S.; Christian, J.; Warren, B.; Roberts, S. A.; Harris, S. J.; Perry, D. L. Cryogenic Electron Microscopy Reveals That Applied Pressure Promotes Short Circuits in Li Batteries. Iscience 2021, 24(12). 6) Harrison, K. L.; Goriparti, S.; Merrill, L. C.; Long, D. M.; Warren, B.; Roberts, S. A.; Perdue, B. R.; Casias, Z.; Cuillier, P.; Boyce, B. L. Effects of Applied Interfacial Pressure on Li-Metal Cycling Performance and Morphology in 4 M LiFSI in DME. ACS Applied Materials & Interfaces 2021, 13(27), 31668-31679.

batteries↗
DOE OSTI2024

Detection and Signal Processing for Near-Field Nanoscale Fourier Transform Infrared Spectroscopy

Researchers from a broad spectrum of scientific and engineering disciplines are increasingly using scattering-type near-field infrared spectroscopic techniques to characterize materials non-destructively with nanoscale spatial resolution. However, a sub-optimal understanding of a technique's implementation can complicate data interpretation and act as a barrier to entering the field. Here the key detection and processing steps involved in producing scattering-type near-field nanoscale Fourier transform infrared spectra (nano-FTIR) are outlined. The self-contained mathematical and experimental work derives and explains: i) how normalized complex-valued nano-FTIR spectra are generated, ii) why the real and imaginary components of spectra qualitatively relate to dispersion and absorption respectively, iii) a new and generally valid equation for spectra which can be used as a springboard for additional modeling of the scattering processes, and iv) an algebraic expression that can be used to extract an approximation to the sample's local extinction coefficient from nano-FTIR. The algebraic model for weak oscillators is validated with nano-FTIR and attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectra on samples of polystyrene and Kapton and further provides a pedagogical pathway to cementing some of the technique's key qualitative attributes.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Data Analysis, Machine Learning, & More

At LANL, I have had the privilege and pleasure of working with Dr. Tika Kafle, an optics and condensed matter physicist at the MagLab in TA-35. Dr. Kafle’s research primarily involves the Angle Resolved Photoemission Spectroscopy (ARPES) technique of characterizing materials. More specifically, Dr. Kafle works with Time Resolved ARPES (Tr-ARPES), which extends this technique into the time domain.

36 MATERIALS SCIENCE↗
NASA NTRS1993

Material characterization and modeling with shear ography

Shearography has emerged as a useful technique for nondestructible evaluation and materials characterization of aerospace materials. A suitable candidate for the technique is to determine the response of debonds on foam-metal interfaces such as the TPS system on the External Tank. The main thrust is to develop a model which allows valid interpretation of shearographic information on TPS type systems. Confirmation of the model with shearographic data will be performed.

Workman, Gary L.↗
DOE OSTI2026

A Review of Advanced Characterization Methods and Techniques for Amorphous and Poorly Crystalline Materials Applicable to Cementitious Waste Forms

This review covers advanced characterization methods of cementitious materials. The particular focus is to understand cementitious compositions with amorphous content because conventional techniques such as X-ray diffraction are more applicable to materials with long range order. Also of interest is advanced characterization that provides deeper insights into properties such as porosity. There are five groups of characterization methods discussed in this review which are: electron beam/microscopy, X-ray, neutron diffraction and scattering, nuclear magnetic resonance, and optical techniques. The techniques can be further grouped by the categories of nanoscale structural understanding (transmission electron microscopy and pair distribution function), microscale structural understanding (focused ion beam and x-ray tomography), microscopic elemental distributions (energy dispersive spectroscopy and X-ray fluorescence), and chemical binding information (electron energy loss spectroscopy, x-ray absorption spectroscopy, nuclear magnetic resonance, Raman spectroscopy, and infrared spectroscopy), with advantages and disadvantages of each method discussed. The recommendation for further research is to begin with techniques that are easier to prepare samples for, measure, and analyze, such as the optical techniques of Raman and infrared spectroscopy. If more information is needed, pursue collaborations, other techniques, or proposals for beam time at the synchrotron sources.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS1980

Quantitative ultrasonic evaluation of engineering properties in metals, composites and ceramics

Ultrasonic technology from the perspective of nondestructive evaluation approaches to material strength prediction and property verification is reviewed. Emergent advanced technology involving quantitative ultrasonic techniques for materials characterization is described. Ultrasonic methods are particularly useful in this area because they involve mechanical elastic waves that are strongly modulated by the same morphological factors that govern mechanical strength and dynamic failure processes. It is emphasized that the technology is in its infancy and that much effort is still required before all the available techniques can be transferred from laboratory to industrial environments.

Vary, A.↗
DOE OSTI2024

Covalent integration of polymers and porous organic frameworks

Covalent integration of polymers and porous organic frameworks (POFs), including metal-organic frameworks (MOFs), covalent organic frameworks (COFs) and hydrogen-bonded organic frameworks (HOFs), represent a promising strategy for overcoming the existing limitations of traditional porous materials. This integration allows for the combination of the advantages of polymers, i.e., flexibility, processability and chemical versatility etc., and the superiority of POFs, like the structural integrity, tunable porosity and the high surface area, creating a type of hybrid materials. These resulting polymer-POF hybrid materials exhibit enhanced mechanical strength, chemical stability and functional diversity, thus opening up new opportunities for applications across a large variety of fields, such as gas separation, catalysis, biomedical applications, environmental remediation and energy storage. In this review, an overview of synthetic routes and strategies on how to covalently integrate different polymers with various POFs is discussed, especially with a particular focus on methods like polymerization within, on and among POF structures. To investigate the unique properties and functions of these resultant hybrid materials, the characterization techniques, including nuclear magnetic resonance spectroscopy (NMR), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), transmission electron microscopy (TEM) and scanning electron microscopy (SEM), gas adsorption analysis (BET) and computational modeling and machine learning, are also presented. The ability of polymer-POFs to manipulate the pore environments at the molecular level affords these materials a wide range of applications, providing a versatile platform for future advancements in material science. Looking forward, to fully realize the potential of these hybrid materials, the authors highlight the scalability, green synthesis methods, and potential for stimuli-responsive polymer-POF materials as critical areas for future research.

Hossain, Md Amjad↗
NASA NTRS1980

Quantitative ultrasonic evaluation of engineering properties in metals, composites, and ceramics

Ultrasonic techniques that have demonstrated potential for material characterization are reviewed. These techniques rely on physical acoustic properties of materials and the interaction of elastic stress waves with morphological factors in the ultrasonic regime. The speed of wave propagation and energy loss by interaction with material microstructure and geometrical factors underlie ultrasonic determination of material properties. Two categories of ultrasonic measurements are discussed: those related to material strengths (e.g., elastic moduli, tensile strength, and fracture toughness) and those related to morphology and material conditions that govern strength and performance (e.g., microstructure, void content, residual stress, fatigue damage). It is shown that large-scale industrial application of ultrasonic NDE will depend on advancement in such areas as theory development, instrumentation, system automation, standardization, and coordination with design.

Vary, A.↗
NASA NTRS1983

A study of the stress wave factor technique for the characterization of composite materials

A testing program was undertaken to provide an independent investigation and evaluation of the stress wave factor for characterizing the mechanical behavior of composite laminates. Some of the data which was obtained after performing a very large number of tests to determine the reproducibility of the SWF measurement is presented. It was determined that, with some optimizing of experimental parameters, the SWF value can be reproduced to within + or - 10%. Results are also given which show that, after careful calibration procedures, the lowest SWF value along the length of a specimen will correlate very closely to the site of final failure when the specimen is loaded in tension. Finally, using a moire interferometry technique, it was found that local regions having the highest in plane strains under tensile loading also had the lowest SWF values.

Henneke, E. G., II↗
DOE OSTI2025

Protecting air/moisture-sensitive samples using perdeuterated paraffin wax for solid-state NMR experiments under magic-angle spinning

Solid-state nuclear magnetic resonance (SSNMR) spectroscopy is a powerful technique for materials characterization, yet its application to air- and moisture-sensitive materials is often hindered by the difficulty in maintaining an inert environment during magic-angle spinning (MAS). This is particularly true for fast-MAS rotors that do not generally provide tight seals. Herein, we present a generalizable approach employing perdeuterated paraffin waxes—n-icosane-d42 and c-dodecane-d24—as protective embedding media to analyze sensitive organometallic catalysts using SSNMR. We demonstrate that these waxes significantly slow oxidative degradation under MAS conditions. Weak background 1 H and 13 C NMR signals from the waxes are effectively suppressed using double-quantum filtration and cross-polarization techniques. In conclusion, these findings offer a robust method for expanding the scope of SSNMR to air-sensitive systems, with implications for the structural study of reactive materials and catalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Microstructure Clones

Background: A material’s microstructure drives its material performance. Contemporary crystal plasticity experiments compare full-field strain measurements of polycrystal specimens to models. Because each specimen is unique, it is impossible to know which features of the observed deformation are deterministic vs statistical; thus, differences between model and experiment may or may not be significant. Objective: This paper introduces the invention of microstructure clones. Microstructure clones are 2D oligocrystal specimens that have nearly identical microstructures to remedy the aforementioned experimental limitations. Having specimens with nearly identical microstructures will allow for multiple destructive tests of a microstructure (either as repeats or intentionally different experiments), an ability to “see the future” by providing insight into how a specimen will deform, variability quantification, and experimental investigations of response to small microstructural changes. Methods: This work introduces microstructure clones. Repeatability of these clones is demonstrated in tensile bars of pure nickel. Local strain measurements from digital image correlation are compared between clone specimens and compared to results from a crystal plasticity finite element model. Results: Two sets of microstructure clones were tested in this study and displayed very consistent deformation responses within each clone set. Small observed differences in deformation invite investigation into microstructure stochasticity and the effect of small microstructural and loading differences. Conclusions: Microstructure clones represent a significant shift in understanding structure–property relationships. This work reshapes experimental crystal plasticity to allow for experiments that control for specific variables, quantification of microstructural stochasticity (and other sources of stochasticity), and opportunities for replicating experiments.

Crystal Plasticity↗
DOE OSTI2024

Open-Source Data Analysis Tool for Spectral Small-Angle X-ray Scattering Using Spectroscopic Photon-Counting Detector

Spectral small-angle X-ray scattering (sSAXS) is a powerful technique for material characterization from thicker samples by capturing elastic X-ray scattering data in angle- and energy-dispersive modes at small angles. This approach is enabled by the use of a 2D spectroscopic photon-counting detector that provides energy and position information of scattered photons when a sample is irradiated by a polychromatic X-ray beam. Here, we describe an open-source tool with a graphical interface for analyzing sSAXS data obtained from a 2D spectroscopic photon-counting detector with a large number of energy bins. The tool takes system geometry parameters and raw detector data to output 1D scattering patterns and a 2D spatially-resolved scattering map in the energy range of interest. We validated these features using data from samples of caffeine powder with well-known scattering peaks. This open-source tool will facilitate sSAXS data analysis for various material characterization applications.

Chemistry↗
NASA NTRS2002

Ultrasonic Resonance Spectroscopy of Composite Rims for Flywheel Rotors

Flywheel energy storage devices comprising multilayered composite rotor systems are being studied extensively for utilization in the International Space Station. These composite material systems were investigated with a recently developed ultrasonic resonance spectroscopy technique. The ultrasonic system employs a continuous swept-sine waveform and performs a fast Fourier transform (FFT) on the frequency response spectrum. In addition, the system is capable of equalizing the amount of energy at each frequency. Equalization of the frequency spectrum, along with interpretation of the second FFT, aids in the evaluation of the fundamental frequency. The frequency responses from multilayered material samples, with and without known defects, were analyzed to assess the capabilities and limitations of this nondestructive evaluation technique for material characterization and defect detection. Amplitude and frequency changes were studied from ultrasonic responses of thick composite rings and a multiring composite rim. A composite ring varying in thickness was evaluated to investigate the full thickness resonance. The frequency response characteristics from naturally occurring voids in a composite ring were investigated. Ultrasonic responses were compared from regions with and without machined voids in a composite ring and a multiring composite rim. Finally, ultrasonic responses from the multiring composite rim were compared before and after proof spin testing to 63,000 rpm.

Harmon, Laura M.↗
DOE OSTI2024

Characterization Techniques Investigated for Characterization of Anomalous Materials in Plutonium Oxide – 25666

The DOE has adopted a Dilute and Dispose approach for processing surplus plutonium which consists of blending plutonium oxide with adulterants and packaging it in a form which is acceptable for disposal at the Waste Isolation Pilot Plant. The feed material for the downblend process is intended to be pure plutonium oxide powder, however other objects are occasionally encountered within the oxide, particularly with legacy material. Potential technologies which could assist in the resolution of incidents where such anomalies are encountered have been investigated. Resolution of these incidents requires characterization of the anomalous object so that plutonium oxide processing can resume and so that a disposition pathway can be determined for the anomalous material. Technologies including gamma ray spectroscopy, alpha-gamma coincidence, LiDAR volumetric measurements, and surface conductivity measurements were investigated for this purpose, with a focus on systems which can be easily introduced into the processing environment when an anomaly is encountered, then removed from the environment after resolution to avoid impeding normal processing activities. This places an emphasis on small and portable measurement systems and systems that can operate in a high-background, oxide-processing environment. Gamma ray systems investigated include the GR1™a CZT detector and the MicroGe™a germanium detector, with a focus on detecting characteristic gamma rays from Pu-239 and other actinides. A gamma ray and alpha particle coincidence method was investigated with the goal of identifying actinides in the presence of a gamma ray background produced by adjacent plutonium oxide material. Leica™b BLK360 G1 and Keyence™c LJ-X8300 LiDAR systems were investigated for use in conjunction with mass measurements to gain accurate material density values, and a Foerster Sigmatest™d 2.070 was tested to determine surface conductivity. The combination of these properties would allow improved identification and characterization of a wide variety of potential anomalous material.

Munson, Justin M.↗
DOE OSTI2025

Smaller and faster: a review of conventional and nanocalorimetry techniques for determining thermophysical properties of nuclear materials

Thermal analysis of nuclear materials is critical for the advancement of nuclear technology. The heat effects associated with heat capacity, phase transformation, and radiation damage can be measured with conventional calorimeters. However, conventional calorimetric techniques are often restricted in terms of heating rate and sample mass, especially when studying the limited amounts of materials subject to extreme conditions. In this review, we summarize conventional calorimetric studies of critical thermophysical and thermochemical properties of pure actinide metals (U, Np, Am, Pu), fast reactor metallic fuel alloy systems (U–Zr, U–Pu–Zr, Pu–U, Pu–Zr), and actinide oxides that are primary constituents or transmutation products in light water reactor fuel rods (U–O, Np–O, Am–O, Pu–O, Pu–U–O). Adiabatic and drop calorimetry have been the primary techniques used for these studies, however the development of fast scanning calorimetry using micro-electro-mechanical-based systems allows determination of thermodynamic properties from smaller sample masses. We report recent investigations that leverage the fast heating rates of nanocalorimetry by itself or combined with other characterization techniques. Furthermore, we then discuss opportunities for nanocalorimetry to provide solutions to some of the technical challenges inherent in thermal analysis of nuclear materials, namely a reduction in sample activity, emulating heating transients, investigation of phase evolution in irradiated samples, and characterization of radiation damage evolution. Nanocalorimetry has the potential to significantly advance the understanding of thermophysical properties in nuclear materials and thus accelerate the development of nuclear technology.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗