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Results for “phase characterization”

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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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Solid phase characterization and transformation of illite mineral with gas-phase ammonia treatment

In situ remediation applications of ammonia (NH 3 ) gas have potential for sequestration of subsurface contamination. Ammonia gas injections initially increase the pore water pH leading to mineral dissolution followed by formation of secondary precipitates as the pH is neutralized. However, there is a lack of understanding of fundamental alteration processes due to NH 3 treatment. In these batch studies, phyllosilicate minerals (illite and montmorillonite) were exposed to NH 3 gas with subsequent aeration to simulate in situ remediation. Following treatments, solids were characterized using a variety of techniques, including X-ray diffraction, N 2 adsorption-desorption analysis for surface area, Fourier transform infrared (FTIR) spectroscopy, nuclear magnetic resonance (NMR), and microscopy methods to investigate physicochemical transformations. The results of this study indicate that, at high pH, the clays are altered as observed by differences in morphology and particle size via microscopy. However, the two clays interact differently with NH 3 . While montmorillonite interlayers collapsed due to intercalation, illite layers were unaffected as confirmed by FTIR analysis. Further, structural changes in silicate ([SiO 4 ] n- ) and aluminol (Al-OH) groups were identified by NMR and FTIR. This research showed that mineral alteration processes occur during and after NH 3 gas treatment which may be used to remove radionuclides from the aqueous phase through sorption, co-precipitation, and coating with secondary phyllosilicate alteration products.

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

Multi-phase characterization of pitch-carbon coated nano-silicon anodes for lithium-ion batteries

Silicon (Si) is a leading next-generation Li-ion battery anode candidate that meets rigorous performance demands for portable power including enhanced power and energy density with robust cycling performance. However, a series of complex and interrelated reactions lead to reduced calendar life in Si-containing systems and therefore challenge practical adoption. In the present work, we probe the mechanisms underlying observed performance improvements by adding a pitch-carbon coating onto nano-Si material. We pair solid-phase (X-ray photoemission spectroscopy, Fourier-transform infrared), semi-volatile phase (solid-phase microextraction-gas chromatography-mass spectrometry), and gas-phase (gas chromatography-flame-ionization detector) characterization signals to comprehensively evaluate the impact of pitch-carbon coating on the evolution of the Si solid-electrolyte interphase (SEI) and the associated impacts on electrode/electrolyte reactivity. The pitch-carbon is found to serve as a physicochemical barrier, reducing the electro-active surface area for Si/electrolyte reactivity and preventing Si oxidation. Further, the pitch-carbon coating promotes the evolution of a more-favorable SEI by subsuming substantial functionality typically associated with the fluoroethylene carbonate (FEC) electrolyte additive - such as alkoxide scavenging and suppression of transesterification pathways - and by shifting the competitive electrolyte degradation pathways' favorability. The multi-phase characterization approach enables holistic end-products evaluation from complex (electro)chemical interfacial reactions, which informs a robust interpretation of the carbon coating's role in electrochemical performance improvements. The present mechanistic evaluation aids the rational design for improved nano-Si materials.

25 ENERGY STORAGE↗
DOE OSTI2021

Shielded and Low-Damping SPM Probes For Quantitative Electrical and Electrochemical Characterization (Phase IIB)

The purpose of this DOE SBIR award was to develop new scanning probe microscopy tools for the elucidation of electrical and electrochemical properties at the nanoscale. High performance probes are important for energy materials research. In both solar cells and batteries, the essential physics and chemistry occur at the nanoscale and nanoscale characterization tools are required for their elucidation. The introduced new models are a shielded probe and an electrically insulated probe where only less than one micron of a conductive tip is exposed. In Phases I and IIa, we explored the development of cost-effective methods to insulate cantilevers from aqueous solutions and patented a technology that provides an insulated electrical contact to the tip. Also, our technology was adapted to be compatible with all popular commercial AFM systems. In Phase IIb, we improved reproducibility and batch size to drive down costs while maintaining quality control with testing. We transformed our product into a convenient turnkey solution to make electrochemical characterization approachable to a wide range of researchers. In January 2021, the technology was well received by the AFM community and Nanosurf Inc. (Woburn, MA) acquired Scuba Probe Technologies. The technology and expertise of Scuba Probe Technologies complements Nanosurf’s development of the full range of nano-electrical characterization tools.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Beta-Stabilized Ti-5Al-5Mo-5V-3Cr Primary and Secondary Phase Characterization using Ultrasonic Attenuation

Ti-5Al-5Mo-5V-3Cr (Ti-5553) is a beta-stabilized titanium alloy being evaluated for its use in additive manufacturing. The development of effective nondestructive characterization tools will be critical for successful insertion of Ti-5553 into applications. The microstructure of Ti-5553 can be modified significantly, through heat treatments alone, to produce single β-phase microstructure or dual α-β microstructure with variations on the types and quantities of the α phase in a β matrix. In this work, a set of heat treatments was chosen to obtain a range of microstructures, followed by an investigation of the ultrasonic response to gauge the degree to which these variations could be detected. Ultrasonic attenuation was selected because of its ability to detect differences in grain size and, potentially, the existence and limited details of secondary phases . Initial results show a very distinctive difference in attenuation between the single phase β and the α+β microstructures, and smaller, but still significant, differences among the α+β microstructures indicating that this approach merits further development.

ultrasonic attenuation, Ti-5Al-5Mo-5V-3Cr, heat tr↗
DOE OSTI2022

TEM-based phase characterization of $\mathrm{U–19Pu–10Zr}$ irradiated in ATR

We report the results of the microstructural examination of the irradiated U–19Pu–10Zr fuel. New insights gained using selective area electron diffraction analysis in a transmission electron microscope provide crystallographic information on the phases previously identified based primarily on the chemical compositions. After irradiation, the microstructure of the fuel separates into γ-(U, Pu, Zr) in the central region with a secondary nanocrystalline UO 2 phase, γ-(U, Pu, Zr) with a secondary ZrO 2 phase in the intermediate, and ζ-(U, Pu) in the outer regions. While the surface microstructural features and porosity indicate separation into three concentric zones consistent with the existing constituent redistribution model, crystallographically the fuel consists of two zones: inner (with γ-(U, Pu, Zr) as a matrix phase) and outer (with ζ-(U, Pu) as a matrix phase). Our results highlight the importance of crystal structure in phase identification and can be used to supplement the existing constituent redistribution model.

extreme environment↗
DOE OSTI2025

Carrier-envelope-phase characterization of ultrafast mid-infrared laser pulses through harmonic generation and interference in argon

The propagation of an intense, femtosecond, mid-infrared laser pulse in a gaseous medium results in the efficient generation of spectrally overlapping low-order harmonics, whose optical carrier phases are linked to the carrier-envelope phase (CEP) of the mid-infrared driver pulse. Random peak-power fluctuations of the driver pulses, converted to the fluctuations of the nonlinear phases, acquired by the pulses on propagation, cause this phase correlation to smear out. We show that this seemingly irreversible loss of phase can be recovered, and that the complete information needed for the phase correction is contained in the harmonic spectra itself. The optical phases of the intense driver pulse and its harmonics, as fragile as they appear to be against even weak disturbances, evolve deterministically during highly nonlinear propagation through the extended ionization region.

nonlinear optics↗
DOE OSTI2021

Shielded and Low-Damping SPM Probes for Quantitative Electrical and Electrochemical Characterization (Phase IIA)

The purpose of this DOE SBIR award was to develop new scanning probe microscopy tools for the elucidation of electrical and electrochemical properties at the nanoscale. High performance probes are important for energy materials research. In both solar cells and batteries, the essential physics and chemistry occur at the nanoscale and nanoscale characterization tools are required for their elucidation. Two products were developed: an electrically shielded probe and an electrically conductive probe with low leakage currents. Our processes were based on post processing of existing probes and fabrication methods were tested, leading to a laser micromachining based approach that led to the first minimal viable product. We invented a method to make a reliable electrical contact that attaches a flexible printed circuit board to the chip. enable leak-free operation crucial when used in conductive liquids and electrolytes. This proprietary solution improves chip handling, reduces contamination, and maintains effective electrical contact. The probes fabricated in this Phase IIa are a minimal viable product which attracted attention from various tip manufacturers and instrument manufacturers alike.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Evaluating Contributions of Pitch-Carbon Coating to Improved Stability of Si Anodes Through Voltage-Resolved Multi-Phase Characterization

Silicon nanoparticles have emerged as a promising alternative to graphite to improve the energy density of next-generation lithium-ion battery anodes. Nano-sized Si domains facilitate rapid ion transport and minimize particle-scale mechanical degradation, but also exhibit increased (electro)chemical reactivity with Li-ion electrolyte components due to their high surface area. We have previously demonstrated that surface modification of Si nanoparticles with pitch-carbon is an effective strategy to reduce these parasitic reactions. In the present work, we holistically evaluate the mechanistic contribution of pitch-carbon coating to the observed stability improvement over uncoated Si. We utilize coupled in situ and ex situ methods to probe changes to solid-surface, volatile headspace, and gas-phase chemistry occurring during initial cycling. Measurements taken at targeted potentials associated with electrolyte species reduction enables the decoupling of specific reaction pathways tied to interfacial stability. Further, we demonstrate the non-trivial role of gas reconsumption in dictating the nature of the passivating surface layer evolved on both uncoated and pitch-coated Si. This multi-phase analysis offers insights into the mechanism of effective surface passivation, which may be applied to inform future Si material development.

ENERGY STORAGE↗
DOE OSTI2024

SRNL High and Low Activity Residue Characterization System Phase II [Poster]

The characterization system contains data sampled from 1996 to 2024 and can display any desired combination of 45 different isotopes. This system is intended to be used to quickly access historical data, generate trends for accurate future projections, and evaluate relevant unit conversion calculations.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2026

Multiscale characterization of phase change materials for building thermal energy storage applications

Phase change materials (PCMs) store and release large amounts of thermal energy because of their high latent energy storage capacity. However, long-term cyclic stability, supercooling and performance-scalability are some of the major challenges for their use in building thermal energy storage (TES) applications. Here, in this study, we present a comprehensive multiscale characterization of two commercially available organic PCMs, Puretemp 18 and Puretemp 23. At the microscale, differential scanning calorimetry (DSC) was used to characterize phase change temperature, specific heat, and latent heat. At the mesoscale, a heat flow meter apparatus (HFMA), following the ASTM C1784 standard, was employed to measure the phase change temperature, specific heat, and latent heat properties. A comparative analysis of latent heat as a function of temperature was conducted by integrating the DSC and HFMA results. At the macroscale, the thermal performance and cyclic stability of the TES system was evaluated using Puretemp 23. The TES system consisted of a finned tube heat exchanger with a storage volume of 0.0189 m 3 (5 gal), which represents a compact, real-world TES solution suitable for building energy storage. The results showed consistent thermal stability of the PCM over 200 cycles, and the supercooling temperature remained within 0.2 °C, which was not detected in smaller-scale characterization methods. Additionally, the macroscale testing methodology of the PCM revealed that the TES is able to charge and discharge stored latent energy within 2 h under a temperature differential of 16.67 °C measured between the inlet water temperature and the phase transition temperature of the PCM. The proposed multiscale PCM characterization method provides a systematic basis for comparing important thermal storage properties while also investigating the scalability, reliability and integration challenges in large scale TES applications.

Latent heat↗
DOE OSTI2023

Analysis of neptunium oxides produced through modified direct denitration

Production of neptunium-237 ( 237 Np) target materials for plutonium-238 ( 238 Pu) radioisotope thermoelectric generators (RTGs) for deep space exploration requires advanced chemistry and engineering development. Currently, the domestic Pu-238 Supply Program at Oak Ridge National Laboratory produces neptunium dioxide (NpO 2 ) for target material using a modified direct denitration (MDD) flowsheet. Although the chemistry, reaction mechanisms, and product characteristics of MDD are well understood for uranium, corresponding studies of the neptunium system are still needed to continue optimization of target material properties, production equipment design, and production flowsheets. Here, the objective of this work is to characterize crystalline phases, morphology, surface texture, and particle size of NpO 2 produced via MDD reactions. Solid-phase characterization techniques, including powder X-ray diffraction (pXRD) and scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS), were employed to achieve this objective. Subsequent data processing using the Morphological Analysis for Material Attribution (MAMA) software was performed to analyze particle morphology and size. Broadly, the powders were found to contain a mixture of NpO 2 and Np 2 O 5 after denitration with a variety of morphologies. After high-firing, the product was found to be NpO 2 with a typical polycrystalline oxide morphology and a grain size ranging from 0.72 to 0.94 µm. These analyses provide knowledge on the reaction pathway for a non-traditional NpO 2 synthesis method and offer additional unique insight into production-scale environments for transuranic materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

In Situ High Energy X-ray Diffraction Characterization of Phase Transformations and Mechanical Behaviors in Rapidly Solidified Titanium and Stainless Steel Alloys [Thesis]

Advanced manufacturing techniques like additive manufacturing (AM) have poised themselves to revolutionize metal manufacturing. A wide range of AM techniques are capable of manufacturing metal components with unique, complex geometries and hastening the scientific-engineering-development cycle. Metal AM relies on a layer-by-layer rapid manufacturing process to build components from the substrate up. Rapid solidification is a large departure from traditional metal manufacturing due to its complex physics. Characterization of rapid solidification is difficult, stemming from the small volumes used in AM and the fast dynamics of the process. High energy X-ray diffraction (HEXRD) is a solution to the characterization problems of rapidly solidified alloys and AM. HEXRD can probe small volumes at fast rates and provides a wide range of thermomechanical and kinetic information. This thesis presents the application of HEXRD to rapidly solidified titanium and stainless steel alloys through a series of case studies. In the first two studies, HEXRD is applied to rapidly solidified titanium and stainless steel welds. The materials are characterized for their temperature history, phase changes, kinetics, and microstructural evolution. In the next case study, HEXRD is applied to characterize phase changes in elastocaloric NiTi shape memory alloys (SMAs) under thermomechanical load. HEXRD, in conjunction with other tools, is used to explain the superior performance of the additively manufactured SMAs. In the final two case studies, HEXRD is used to measure the mechanical response of AM parts with complex geometries; namely, the octet truss lattice. Diffraction reveals a wide range of materials information about the AM microstructure including unexpected phases, texture, and mechanical response to loading. The mechanical results from HEXRD and then compared with theoretical predictions about the performance of octet truss lattices. Summarily, HEXRD is a diverse tool that is poised to address the complex characterization problems of many aspects of the additive manufacturing process.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Transmission electron microscopy study of a high burnup U-10Zr metallic fuel

To support the development of U-10 wt.% Zr (U-10Zr) metallic fuel for Gen IV sodium-cooled fast reactors, we analysed a solid, Na-bonded, U-10Zr (by weight percent) fuel cross section that was irradiated to a burnup of ~ 12.4 % at.% at the Fast Flux Test Facility (FFTF). Advanced characterization techniques, including site specific sample preparation by focused ion beam (FIB) and phase/chemical determination by transmission electron microscopy (TEM), were used to reveal the constituent redistribution of Zr, characterize the fuel phases and the secondary phases (such as solid fission products) present at the end of life. It is shown that the fuel pin cross section is divided into three major concentric zones: a Zr-rich central region, a Zr-lean intermediate region, and a Zr intermediate peripherical region. The phase characterization revealed that the irradiation environment enhanced the development and stabilization of phases not predicted by the standard equilibrium U-Zr phase diagrams. Comparing the current results with the ones from previous studies, it is reaffirmed that the irradiation temperature and the time spent in the reactor, rather than the fuel burnup, are the two factors that most influence the formation of redistribution zones and their extension along the fuel cross section. Various solid fission products precipitated inside the fission gas pores, such as lanthanides, ZrRu, BaTe, CsI, and Ba and Sr oxides. Here, this study provides unprecedented nanoscale understandings in the U-10Zr fuel system that may benefit fuel performance modelling and advanced fuel development.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Thermal property characterization of phase change materials in building applications: A systematic review of fundamentals, recent progress, and future directions

Phase change materials (PCMs) can reduce building peak loads and enable demand-responsive thermal energy storage (TES), but their deployment depends on reliable measurement and interpretation of thermal properties across laboratory, intermediate, and application scales. Here, this review systematically examines characterization methods, testing protocols, and recent advances for neat PCMs and PCM composites, emphasizing thermal conductivity, enthalpy-related properties (phase change temperature, latent heat, specific heat), and cycling stability. For thermal conductivity, we compare steady-state and transient techniques and note limitations when phase transition and contact resistance affect measurements. For enthalpy–temperature characterization, we discuss differential scanning calorimetry together with intermediate- and bulk-scale methods, including T-history, heat flow meter testing, and three-layer calorimetry (3LC), to generate application-relevant enthalpy–temperature profiles. Cycling stability is organized into four experimental families: thermoelectric–air, fully thermoelectric, water-bath, and in situ chamber approaches, with attention to separating reversible supercooling from true degradation such as phase segregation. We highlight emerging noncontact diagnostics, including infrared thermography and embedded sensing, for spatially resolved validation and multiscale interpretation. Finally, we review the growing use of AI and machine learning for property prediction, inverse characterization from experimental signals, and real-time state estimation in building-integrated TES. Key needs include harmonized protocols, interlaboratory benchmarking, uncertainty reporting, and metadata-rich datasets to accelerate reproducible PCM qualification for grid-flexible buildings.

AI↗
DOE OSTI2022

In situ characterization of phase transformations in petroleum pitch by high temperature X-ray diffraction

The phase transformation from isotropic to mesophase of a petroleum-derived pitch was monitored by in situ X-ray diffraction at 410 °C. The kinetics of the transformation were characterized by monitoring the growth of a broad peak at 2θ~24° and could be described by Avrami’s equation. The volatilization of low molecular weight components originally present in the pitch, or produced during the condensation reaction, was assessed by thermal gravimetry analysis, following the same thermal history. Ex situ characterizations of the pitch precursor before and after thermal treatment provided insight into the evolution of the molecular structure associated with mesophase generation (optical polarized microscopy, molecular weight distribution by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, X-ray photoelectron spectroscopy, Auger spectroscopy, and thermal stability). Here, this investigation demonstrates the value of using complementary in situ and ex situ experimental techniques to characterize complex mechanisms during the processing of organic materials.

02 PETROLEUM↗
DOE OSTI2024

An Investigation of Oxides of Tantalum Produced by Pulsed Laser Ablation and Continuous Wave Laser Heating

Recent progress has seen multiple Ta 2 O 5 polymorphs generated by different synthesis techniques. However, discrepancies arise when these polymorphs are produced in widely varying thermodynamic conditions and characterized using different techniques. This work aimed to characterize and compare Ta 2 O 5 particles formed at high and low temperatures using nanosecond pulsed laser ablation (PLA) and continuous wave (CW) laser heating of a local area of tantalum in either air or an 18 O 2 atmosphere. Scanning electron microscopy (SEM) and Raman spectroscopy of the micrometer-sized particles generated by PLA were consistent with either a localized amorphous Ta 2 O 5 phase or a similar, but not identical, crystalline β-Ta 2 O 5 phase. The Raman spectrum of the material formed at the point of CW laser impingement was in good agreement with the previously established ceramic “H-Ta 2 O 5 ” phase. TEM and electron diffraction analysis of these particles indicated the phase structure matched an oxygen-vacated superstructure of monoclinic H-Ta 2 O 5 . Further from the point of laser impingement, CW heating produced particles with a Raman spectrum that matched β-Ta 2 O 5 . We confirmed that the high-temperature ceramic phase characterized in previous work by Raman spectroscopy was the same monoclinic phase characterized in different work by TEM and could be produced by direct laser heating of metal in air.

36 MATERIALS SCIENCE↗