Search NASASearch

SEARCH · Search NASA

Results for “phase identification”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 37 records · Page 2

Ice Phase Classification Made Easy with Score-Based Denoising

Accurate identification of ice phases is essential for understanding various physicochemical phenomena. However, such classification for structures simulated with molecular dynamics is complicated by the complex symmetries of ice polymorphs and thermal fluctuations. For this purpose, both traditional order parameters and data-driven machine learning approaches have been employed, but they often rely on expert intuition, specific geometric information, or large training data sets. In this work, we present an unsupervised phase classification framework that combines a score-based denoiser model with a subsequent model-free classification method to accurately identify ice phases. Further, the denoiser model is trained on perturbed synthetic data of ideal reference structures, eliminating the need for large data sets and labeling efforts. The classification step utilizes the smooth overlap of atomic position (SOAP) descriptors as the atomic fingerprint, ensuring Euclidean symmetries and transferability to various structural systems. Our approach achieves a remarkable 100% accuracy in distinguishing ice phases of test trajectories using only seven ideal reference structures of ice phases as model inputs. This demonstrates the generalizability of the score-based denoiser model in facilitating phase identification for complex molecular systems. The proposed classification strategy can be broadly applied to investigate structural evolution and phase identification for a wide range of materials, offering new insights into the fundamental understanding of water and other complex systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

A critical analysis of U-Pu-Zr phase transitions using calorimetric, microstructural, and phase equilibria data

Metallic fuels consisting primarily of uranium, plutonium, and zirconium (U-Pu-Zr) are a leading material candidate for fast-spectrum nuclear reactors. Early demonstration programs proved the principle of safe and efficient fast reactor operation, however there is still considerable uncertainty regarding the phase equilibria and microstructural evolution across the ternary composition space. Quantitative phase formation and identification measurements are scarce and often incomplete, with studies reporting either phase transition temperatures or phase identification data, but not both from the same specimens. In this study, we critically compared experimental and calculated phase transition data and correlated with the microstructure and phase characterization data of as-cast and annealed U-Pu-Zr alloys. Differential scanning calorimetry (DSC) was used to measure phase transitions in the subsolidus regions (723−948 K) of three ternary U-Pu-Zr alloys with similar plutonium concentrations but various U/Zr ratios. Due to sluggish kinetics and narrow ranges of phase stability, complex peaks required the use of a Frazier-Suzuki peak fitting algorithm to deconvolute and calculate transition peak temperatures and enthalpies. We also identified trends of phase transition behavior by critically comparing our DSC data with previous phase transition measurements as well as historical and calculated phase equilibrium diagrams. In conclusion, this provides a critical approach for benchmarking and assessing the quality of new U-Pu-Zr phase equilibria data prior to its incorporation into nuclear material databases.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Bulk high-temperature superconductivity in pressurized tetragonal La 2 PrNi 2 O 7

The Ruddlesden–Popper (R–P) bilayer nickelate, La 3 Ni 2 O 7 , was recently found to show signatures of high-temperature superconductivity (HTSC) at pressures above 14 GPa . Subsequent investigations achieved zero resistance in single-crystalline and polycrystalline samples under hydrostatic pressure conditions. Yet, obviousdiamagnetic signals, the other hallmark of superconductors, are still lacking owing to the flamentary nature with low superconducting volume fraction. The presence of a new 1313 polymorph and competing R–P phases obscured proper identification of the phase for HTSC. Thus, achieving bulk HTSC and identifying the phase at play are the most prominent tasks. Here we address these issues in the praseodymium (Pr)-doped La 2 PrNi 2 O 7 polycrystalline samples. We find that substitutions of Pr for La efectively inhibit the intergrowth of diferent R–P phases, resulting in a nearly pure bilayer structure. For La 2 PrNi 2 O 7 , pressure-induced orthorhombic to tetragonalstructural transition takes place at P c ≈ 11 GPa, above which HTSC emerges gradually on further compression. The superconducting transition temperatures at 18–20 GPa reach $T$ $^{onset}_{c}$ = $82.5$ $K$ and $T$ $^{zero}_{c}$ = $60$ $K$, which are the highest values, to our knowledge, among known nickelate superconductors. Importantly, bulk HTSC was testified by detecting clear diamagnetic signals below about 75 K with appreciable superconducting shielding volume fractions at a pressure of above 15 GPa. Further, our results not only resolve the existing controversies but also provide directions for exploring bulk HTSC in the bilayer nickelates.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND

Reward Driven Workflows for Unsupervised Explainable Analysis of Phases and Ferroic Variants From Atomically Resolved Imaging Data

Rapid progress in aberration corrected electron microscopy necessitates development of robust methods for the identification of phases, ferroic variants, and other pertinent aspects of materials structure from imaging data. While unsupervised methods for clustering and classification are widely used for these tasks, their performance can be sensitive to hyperparameter selection in the analysis workflow. In this study, the effects of descriptors and hyperparameters are explored on the capability of unsupervised ML methods to distill local structural information, exemplified by the discovery of polarization and lattice distortion in Sm − dopped BiFeO 3 (BFO) thin films. It is demonstrated that a reward-driven approach can be used to optimize these key hyperparameters across the full workflow, where rewards are designed to reflect domain wall continuity and straightness, ensuring that the analysis aligns with the material's physical behavior. This approach allows the discovery of local descriptors that are best aligned with the specific physical behavior, providing insight into the fundamental physics of materials. The reward driven workflow is further extended to disentangle structural factors of variation via an optimized variational autoencoder (VAE). Lastly, the importance of well-defined rewards is explored as a quantifiable measure of the success of the workflow.

Barakati, Kamyar [University of Tennessee, Knoxvil

What Is the Limit of Quantification for the Minor Phase in Time-of-Flight Neutron Diffraction? A Case Study on Fe and Ni Powder Mixtures at VULCAN

A phase present in small quantities within materials may not simply serve as a secondary component; it can play a crucial role in determining the integrity, properties, and performance of the material. These minor but important phases usually draw attention in material design and processing for fundamental understanding as well as material quality control. Accurately quantifying a minor phase amid a majority phase, especially at extremely low fractions, remains a challenging task. Time-of-flight neutron diffraction, coupled with advanced pattern analysis techniques like Rietveld refinement, is a powerful tool for crystal structure identification and phase quantification. The deep penetrating capability of neutrons enables the detection and quantification of trace phases within materials. In this study, the quantification limits of time-of-flight neutron diffraction were explored using the VULCAN diffractometer at the Spallation Neutron Source, using Fe–Ni powder mixtures as a sample system. By comparing the refinement results to the known weighed values, it was determined that the reliable quantification of a minor Ni phase is achievable down to about 0.1 wt% while a Ni fraction as low as 0.02 wt% is difficult to trace. Effective control of the refinement parameters, especially the profile function parameters, are found to significantly influence the convergence of fittings and the accuracy of phase quantification.

Rietveld refinement

Diffusion and phase formation in the γ-uranium-technetium system

Phase formation in the U-Tc binary system at 800 °C was investigated using a diffusion couple experiment. Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) identified four novel potential intermetallic phases - U 7 Tc 3 , U 13 Tc 12 , U 3 Tc 5 , and UTc 4 . Diffusion coefficients were calculated for the intermetallic phases using the Boltzmann-Matano method and were respectively found to be – 120, 38.2, 15.6, and 1.51 × 10 −18 m 2 /s. Tc also exhibits a solid-solution phase with high penetration into the U with a diffusion coefficient of ∼ 10 −14 m 2 /s. Furthermore, these findings expand the number of known U-Tc phases and provide the first diffusion coefficients for the U-Tc system, and contribute valuable data to the broader field of actinide metallurgy.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Learning to classify quantum phases of matter with a few measurements

We study the identification of quantum phases of matter, at zero temperature, when only part of the phase diagram is known in advance. Following a supervised learning approach, we show how to use our previous knowledge to construct an observable capable of classifying the phase even in the unknown region. By using a combination of classical and quantum techniques, such as tensor networks, kernel methods, generalization bounds, quantum algorithms, and shadow estimators, we show that, in some cases, the certification of new ground states can be obtained with a polynomial number of measurements. An important application of our findings is the classification of the phases of matter obtained in quantum simulators, e.g. cold atom experiments, capable of efficiently preparing ground states of complex many-particle systems and applying simple measurements, e.g. single qubit measurements, but unable to perform a universal set of gates.

quantum machine learning

Temperature-dependent changes in gas chromatographic separation metrics for trihexyl(tetradecyl)phosphonium-based ionic liquid stationary phases and comparison to conventional polysiloxane stationary phases

Here, to assess whether the trihexyl(tetradecyl)phosphonium chloride ([P 66614 + ][Cl - ]) ionic liquid (IL), employed as a gas chromatographic stationary phase, exhibits temperature-dependent phase transitions or structural heterogeneity, retention thermodynamics for probe molecules of varied chemical structure were investigated by gas chromatography (GC) over the temperature range of 25 to 64 °C using van’t Hoff analysis. All van’t Hoff plots for n-alkanes (C8–C12) and other probe analytes were linear, indicating the absence of detectable phase-transition behavior. The [P 66614 + ][Cl - ] IL was further compared with the [P 66614 + ] bis[(trifluoromethyl)sulfonyl]imide ([P 66614 + ][NTf 2 - ]) IL and commercial polysiloxane stationary phases in terms of temperature-dependent resolution behavior and chromatographic selectivity over the temperature range of 28–52 °C. The resolution factors of analytes in mixtures obtained using gas chromatography–mass spectrometry (GC–MS) and the summation of resolution values decreased smoothly with temperature on both IL stationary phases and on the dimethylphenylcyano-substituted polymeric stationary phase (OV-1701), whereas the poly(50% diphenyl/50% dimethyl siloxane) stationary phase (SPB-50) exhibited irregularities in its temperature-dependent summation of resolution profile, showing a distinct maximum in the temperature range of 34–40 °C. Selectivity values for the IL stationary phases were largely determined by the anion, with the [P 66614 + ][Cl - ] IL providing enhanced separation between polar and aromatic analytes, while the [P 66614 + ][NTf 2 - ] IL favored dispersive and π-π interactions that resulted in a reversal of elution order for some aliphatic–aromatic and alkyne-containing analyte pairs. Capillary columns prepared using different surface activation methods and coated with identical [P 66614 + ][Cl - ] IL stationary phase showed indistinguishable temperature-dependent trends in summation of resolution value and selectivity. An evaluation of analyte-specific selectivity provides insight into the characteristic separation behavior of the stationary phases and enables identification of analyte classes that are more efficiently separated on the [P 66614 + ]-based IL stationary phases compared to conventional stationary phase materials.

Chromatographic selectivity

Synthesis of Si-Fe Chondrule-like Dust Analogues in RF Discharge Plasmas

Chondrules are tiny particles that occur in stony meteorites and are considered as the building blocks of early asteroids and planets. It is believed that they were formed by the fast heating of the dust in the solar nebula. To date, there is no lab-scale experimental study of the formation of chondrules from the initial gas phase precursors following fast heating and crystallisation. The motivation of this work is a pre-trial study of the formation of chnodrule-like particles. The formation of meteorites in the space environment is associated with the aggregation of small particles or molecular clouds under the influence of shock waves or high-energy gas discharges in the solar nebula. In this work, the properties of product formation at the nanoscale-level were investigated using different feedstock materials which are the dominant elements in the meteorite. The structural and morphological properties of the synthesised Si-Fe nanomaterials were analysed by scanning/transmission electron microscopy (SEM/TEM), and chemical composition was analysed by X-ray energy-dispersive spectroscopy (EDS). The identification of crystalline phases was carried out by X-ray diffraction (XRD), whereas the presence of an Fe-Si system in the synthesised particles was demonstrated by Mössbauer spectroscopy. The obtained materials were exposed to the relatively high-energy pulsed plasma beam on the substrate with the aim to emulate the possible fast heating and melting of the formed nanoparticles. The formation steps of growing synthetic (engineered) chondro-like particles and nanostructures in laboratory conditions is discussed.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY

Understanding (La,Sr)(Co,Fe)O$_{3-δ}$ Phase Instability within SOECs Using a Combined Experimental and Atomistic Modeling Approach

Understanding the onset of degradation in the air electrode within solid oxide electrolysis cells (SOECs), and the subsequent impact on cell performance, is a critical step in mitigating the performance losses and stability issues of SOECs. In an effort to identify early onset degradation phenomena, SOECs were characterized as fabricated and after testing potentiostatically at 1.3 V for 1000 h at 750 °C. SOEC air electrodes composed of a 1:1 composite of La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3–δ (6428-LSCF) and Gd 0.1 Ce 0.9 O 1.95 (GDC) were studied using synchrotron X-ray diffraction (XRD), scanning transmission electron microscopy coupled with energy dispersive X-ray spectroscopy (STEM-EDS), and X-ray absorption near-edge spectroscopy (XANES) to evaluate the changes in the air electrode structurally and chemically. These techniques show the migration of Sr species from the air electrode through pores in the GDC barrier layer, progressing to the electrolyte boundary, where it accumulates and reacts with (Zr 0.84 Y 0.16 )O 2–δ (YSZ) to form SrZrO 3 . Microscopy results are paired with atomistic simulations to better understand the relationship between the thermodynamic instability of 6428-LSCF and cell fabrication/testing conditions. First-principles calculations reveal that LSCF-6428 is not stable during cell manufacturing and testing conditions, which supports the experimental identification of secondary phases in both as-fabricated and tested cells. Together, these results demonstrate that the challenging environments encountered by SOECs during cell manufacturing and operation lead to instabilities of the target 6428-LSCF anode material and underscore the need for more durable, high-performing SOEC components.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Identification of the glassy state in nanoparticles by transmission electron microscopy

Identification of amorphous phases in nanoparticles by atomic-resolution transmission electron microscopy (TEM) requires analyses such as tilt-angle-dependent TEM imaging and single-nanoparticle electron diffraction, rather than relying on a single TEM image. Here, the disordered structures of amorphous nanoparticles offer unique atomic configurations and properties that differ from the properties of their crystalline counterparts. These characteristics have motivated the exploration of such materials for mechanical, sensing and catalytic applications. In addition, the formation of amorphous metal nanoparticles is an important endeavour to understand the process of vitrification and the nature of the glassy state. Atomic-resolution transmission electron microscopy (TEM) is increasingly being used as a tool for characterizing structures of nanoparticles produced by vitrification. In this Comment, we discuss the pitfalls of using TEM for ascertaining whether nanoparticles are amorphous. We also make recommendations of best practices.

Alcorn, Francis M. [Sandia National Laboratories (

Utah FORGE: RESMAN Well 16A(78)-32 and 16B(78)-32 Stimulation and Circulation Tracer Test Results - 2024

This dataset contains tracer test results from stimulation and circulation experiments conducted on the Utah FORGE wells 16A(78)-32 and 16B(78)-32 during 2024. The data was collected by RESMAN Energy Technology and includes detailed tracer analysis from flowback, short- and extended-duration circulation tests, and reinjection sampling. Sampling included analysis of tracers during different stages of testing in April, August, and September 2024. The dataset is accompanied by an interpretation report and contains time-series tracer concentration data with identification of test phases and sampling conditions. It includes results for flowback from well 16A, commingling effects with water from well 16B, tracer data from short and extended circulation tests, and reinjection tracer corrections for the August/September test. Users should be aware that proprietary tracer methodologies were applied, and they should consult the interpretation report for insights into experimental procedures and data contextualization.

15 GEOTHERMAL ENERGY

Characterization Inform Sustainable Recovery of Critical Minerals from Fossil Energy Waste Feedstocks

Rare earth elements (REE) and other critical minerals (CM, e.g., Co, Ni, Li) have important uses in green energy and modern technologies, yet are vulnerable to potential supply chain disruptions. One potential domestic CM source is fossil energy wastes, such as acid mine drainage (AMD) and treatment solids (AMD solids), coal combustion ash, and Oil and Gas (O&G) drilling wastes (drill cuttings and produced waters). While they can contain lower CM concentrations then traditional ore, the quantity and fast availability as waste feedstock makes them a promising CM resource. To explore their promise, researchers at DOE’s National Energy Technology Laboratory (NETL) have collected and analyzed CM data for aforementioned fossil energy wastes, and utilized advanced geochemical characterization (e.g., synchrotron microprobe and sequential extraction) to identify the CM speciation and binding environments, and developed sustainable and targeted CM recovery. Successful examples include: (1) the discovery of easily mobile REE phases in Ca-rich coal combustion ash and developing a patented REE recovery process from Ca-rich Powder River Basin coal ash; (2) the successful identification of REE/Co/Ni/Zn hosting phases in acid mine drainage treatment solids (AMD solids) with diverse chemical composition (Al, Mn, or Fe-rich) informing the sequential recovery of different REE/CMs from AMD solids; (3) the recovery potential of Li and other CMs in O&G produced waters and drill cuttings. The innovations driven by characterization have the potential to offset the cost of waste management and wastewater treatments while reducing the cost and environmental footprint of CM extraction.

Stuckman, Mengling

Informed Critical Mineral Recovery from Fossil Energy Waste Feedstocks

Critical minerals (CM), such as rare earth elements (REE), cobalt, nickel, and lithium, have important uses in modern energy and technologies, yet are vulnerable to potential supply chain disruptions. One potential domestic CM source is fossil energy wastes, such as coal combustion ash, acid mine drainage (AMD) and treatment solids (AMD solids), and Oil and Gas (O&G) drilling wastes (drill cuttings and produced waters). CM recovery from these feedstocks is promising due to their abundant quantity and fast availability as waste products. To develop informed and effective CM recovery, DOE’s National Energy Technology Laboratory (NETL) have collected and analyzed CM data for aforementioned fossil energy wastes, and utilized advanced geochemical characterization (e.g., synchrotron microprobe, sequential extraction and geochemical modeling) to identify the CM speciation and binding environments. Novel methods that recover multiple CMs while co-producing other valuable byproducts from these feedstocks have been developed. Successful examples include: (1) the discovery of easily mobile REE phases in Ca-rich coal combustion ash resulted in a patented REE recovery process from the ash feedstock while producing zeolite sorbents from the extraction wastes; (2) the successful identification of REE/Co/Ni/Zn hosting phases in acid mine drainage treatment solids (AMD solids) has informed the sequential CM recovery from AMD solids and has inspired lithium sorbent development from the extraction wastes; (3) the recovery potential of Li and other CMs in O&G produced waters and drill cuttings has been explored while the extraction residuals have been demonstrated to support plant growth as soil supplements. The innovations driven by characterization information have the potential to maximize CM recovery revenue, offset the cost of waste management and wastewater treatments while reducing the cost and environmental footprint of CM extraction.

characterization and extraction of rare earth elem

Synthetic Accessibility and Sodium Ion Conductivity of the Na8–x A x P2O9 (NAP) High-Temperature Sodium Superionic Conductor Framework

Advancement of solid-state electrolytes (SSEs) for all solid-state batteries typically focuses on modification of a known structural framework to improve conductivity, e.g., cation substitution for an immobile ion or varying the concentration of the mobile ions. Novel frameworks can be disruptive by enabling fast ion conduction aided by different structure and diffusion mechanisms, thereby unlocking optimal conductors with different properties. Herein, we perform a high-throughput survey of a structural framework for sodium ion conduction, Na8–x A x P2O9 (NAP), to understand the family’s thermodynamic stability, synthesizability, and ionic conduction. We show that the parent phase Na4TiP2O9 (NTP) undergoes a structural distortion (with accompanying conductivity transition) due to unstable phonons arising from pseudo-Jahn–Teller mode in the 1D titanium chains. Screening compounds in which Ti is substituted by other metals computationally reveal a number of candidates that are predicted to be low in formation energy and have high predicted ionic conductivities. High-throughput experimental and subsequent methodology optimization trials deliver one new compound, Na4SnP2O9 (NSP). X-ray diffraction (XRD), microscopy, and spectroscopy characterization indicate that the room-temperature structure of NSP is similar to the high-temperature, orthorhombic NTP phase but with some small unresolved structural differences. These uncharacterized structural details are speculated to limit the ion conductivity. Temperature-dependent XRD and electrochemical impedance spectroscopy indicate multiple coupled conductivity–structure transitions at a high temperature. We demonstrate the challenges with synthesis development and a priori identification of promising SSE phases as a major bottleneck in new (energy) materials development.

Chemical reactions

CNN-Based Phase Fault Classification in Real and Simulated Power Systems Data

This study proposes a convolutional neural network (CNN)–based two-step phase fault detection and identification method to classify anomalies in the power grid signal. Specifically, the first step checks the fault’s existence and determines the need for the second step. Subsequently, in the case of anomalies in the power grid signal, the second step identifies the type of fault, including line-to-line, single-line-to-ground, double-line-to-ground, and triple-line. Accordingly, the CNN architecture is both designed for the classification layers and trained with simulated data. To provide maximum prediction accuracy with minimum processing time, this study investigates the combinations of various feature extraction (FE) techniques, such as fast Fourier transform (FFT), amplitude and phase (AP), auto-correlation function, power spectral density, and wavelet transform (WT). Consequently, simulated and real-world results demonstrate that the proposed two-step method outperforms conventional one-step techniques, with the best performance obtained by using the combination of AP-AP, AP-WT, FFT-AP, and FFT-WT–based FE methods.

Alaca, Ozgur

Error field identification through torque balance on a saturated island in DIII-D

Measurement of the electromagnetic torque on a magnetic island could be an attractive method for error field identification in the early phase of ITER operation. Previous DIII-D experiments (Strait 2014 Nucl. Fusion 54 073004; Shiraki et al 2015 Plasma Phys. Control. Fusion 57 025016) have demonstrated the principle of this approach using a stationary or slowly rotating island, while recent developments in magnetic data analysis (Sweeney and Strait 2019 Phys. Plasmas 26 012509) allow the field of a rapidly rotating island to be readily distinguished from that of the wall currents induced by its rotation. In a recent experiment, a rotating n = 1 magnetic perturbation forced a saturated magnetic island to rotate, thus sampling all toroidal phases periodically in a single discharge. The phase and amplitude of the error field are inferred from analysis of the time-dependent torque balance on the island, including torques from the error field, the applied magnetic perturbation, and the wall currents induced by rotation of the applied perturbation and the island. Furthermore, results agree well with those from more conventional methods.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY