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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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At least 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Solubility Testing to Support the Addition of Sodium Reactor Experiment Material to Sludge Batch 10

The Savannah River Site H-Canyon Facility is planning to discard dissolved Sodium Reactor Experiment (SRE) material into Tank 51 prior to Sludge Batch 10 (SB10). SB10 with the SRE material will be processed in the Defense Waste Processing Facility (DWPF) using the Nitric-Glycolic Acid (NGA) flowsheet. The DWPF Nuclear Criticality Safety Evaluation (NCSE) protects a 14:1 mass ratio of manganese to equivalent uranium-235 in both the solid and liquid phases during processing by requiring a 70:1 mass ratio in the feed. A concern was raised that freshly precipitated manganese in the SRE material will behave differently from the manganese in sludge during DWPF processing and potentially invalidate the criticality control. To mitigate risks to the DWPF criticality controls, the Savannah River National Laboratory (SRNL) performed a metals solubility test applicable to recently precipitated manganese and uranium, as would be expected with SRE transfers to SB10. The objective of this analysis is the tracking of partitioning of the primary fissile component (uranium-235) with the credited poison (manganese) between the aqueous and insoluble phases.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Solid Phase Equilibrium Relations in the CaO-SiO{sub 2}-Nb{sub 2}O{sub 5}-La{sub 2}O{sub 3} System at 1273 K

Silicate slag system with additions Nb and RE formed in the utilization of REE-Nb-Fe ore deposit resources in China has industrial uses as a metallurgical slag system. The lack of a phase diagram, theoretical, and thermodynamic information for the multi-component system restrict the comprehensive utilization process. In the current work, solid phase equilibrium relations in the CaO-SiO{sub 2}-Nb{sub 2}O{sub 5}-La{sub 2}O{sub 3} quaternary system at 1273 K (1000 °C) were investigated experimentally by the high-temperature equilibrium experiment followed by X-ray diffraction, scanning electron microscope, and energy dispersive spectrometer. Six spatial independent tetrahedron fields in the CaO-SiO{sub 2}-Nb{sub 2}O{sub 5}-La{sub 2}O{sub 3} system phase diagram were determined by the Gibbs Phase Rule. The current work combines the mass fraction of equilibrium phase and corresponding geometric relation. A determinant method was deduced to calculate the mass fraction of equilibrium phase in quaternary system according to the Mass Conservation Law, the Gibbs Phase Rule, the Lever’s Rule, and the Cramer Law.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Correlative image learning of chemo-mechanics in phase-transforming solids

We report constitutive laws underlie most physical processes in nature. However, learning such equations in heterogeneous solids (for example, due to phase separation) is challenging. One such relationship is between composition and eigenstrain, which governs the chemo-mechanical expansion in solids. Here we developed a generalizable, physically constrained image-learning framework to algorithmically learn the chemo-mechanical constitutive law at the nanoscale from correlative four-dimensional scanning transmission electron microscopy and X-ray spectro-ptychography images. We demonstrated this approach on Li X FePO 4 , a technologically relevant battery positive electrode material. We uncovered the functional form of the composition–eigenstrain relation in this two-phase binary solid across the entire composition range (0 ≤ X ≤ 1), including inside the thermodynamically unstable miscibility gap. The learned relation directly validates Vegard’s law of linear response at the nanoscale. Our physics-constrained data-driven approach directly visualizes the residual strain field (by removing the compositional and coherency strain), which is otherwise impossible to quantify. Heterogeneities in the residual strain arise from misfit dislocations and were independently verified by X-ray diffraction line profile analysis. Our work provides the means to simultaneously quantify chemical expansion, coherency strain and dislocations in battery electrodes, which has implications on rate capabilities and lifetime. Broadly, this work also highlights the potential of integrating correlative microscopy and image learning for extracting material properties and physics.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Electrochemical Performance of NaFeFe(CN) 6 Prepared by Solid Reaction for Sodium Ion Batteries

Commercially available Na 4 Fe(CN) 6 and Fe 4 [Fe(CN) 6 ] 3 are two cheap compounds that have ever been investigated as positive electrode materials for sodium-ion batteries. However, poor electronic conductivity of Na 4 Fe(CN) 6 and sodium deficiency of Fe 4 [Fe(CN) 6 ] 3 prevent these two materials from being used in practical rechargeable sodium-ion batteries. In this paper, a NaFeFe(CN) 6 cathode material was synthesized by ball milling the Fe 4 [Fe(CN) 6 ] 3 / Na 4 Fe(CN) 6 mixture. The obtained NaFeFe(CN) 6 demonstrated a single cubic phase indexed to Fm3m space group similar to Fe 4 [Fe(CN) 6 ] 3 but with larger lattice parameter due to the existence of Na + in the lattice framework. The NaFeFe(CN) 6 electrode delivered first desodiation capacity of 119.4 mAh g -1 and first sodiation capacity of 153.6 mAh g -1 at 0.05C rate. The NaFeFe(CN) 6 showed excellent cycling stability with reversible capacities of 118.2 mAh g -1 and 96.8 mAh g -1 at 0.1C and 1C rate, respectively. In-situ XRD analyses demonstrated a single cubic phase process during charge-discharge of NaFeFe(CN) 6 electrode. Low water content benefited from the solid reaction method and the homogenous single phase process during charge/discharge assured the stable long term cycling performance of the NaFeFe(CN) 6 product.

25 ENERGY STORAGE↗
DOE OSTI2022

Schmid factor crack propagation and tracking crystallographic texture markers of microstructural condition in direct energy deposition additive manufacturing of Ti-6Al-4V

Metallic additive manufacturing (AM) provides a customizable and tailorable manufacturing process for new engineering designs and technologies. The greatest challenge currently facing metallic AM is maintaining control of microstructural evolution during solidification and any solid state phase transformations during the build process. Ti-6Al-4V has been extensively surveyed in this regard, with the potential solid state and solidification microstructures explored at length. In this study, we evaluate the applicability of previously determined crystallo- graphic markers of microstructural condition observed in electron beam melting powder bed fusion (PBF-EB) builds of Ti-6Al-4V in a directed energy deposition (DED) build process. The aim of this effort is to elucidate whether or not these specific crystallographic textures are useful tools for indicating microstructural conditions in AM variants beyond PBF-EB. Parent β-Ti grain size was determined to be directly related to α-Ti textures in the DED build process, and the solid state microstructural condition could be inferred from the intensity of specific α-Ti orientations. Qualitative trends on the as-solidified β-Ti grain size were also determined to be related to the presence of a fiber texture, and proposed as a marker for as-solidified grain size in any cubic metal melted by AM. Analysis of the DED Ti-6Al-4V build also demonstrated a near complete fracture of the build volume, suspected to originate from accumulated thermal stresses in the solid state. Crack propagation was found to only appreciably occur in regions of slow cooling with large α +β colonies. Schmid factors for the basal and prismatic α-Ti systems explained the observed crack pathway, including slower bifurcation in colonies with lower Schmid factors of both slip systems. Colony morphologies and localized equiaxed β-Ti solidification were also found to originate from build pauses during production and uneven heating of the build edges during deposition. Tailoring of DED Ti-6Al-4V microstructures with the insight gained here is proposed, along with cautionary insight on preventing unplanned build pauses to maintain an informed and controlled thermal environment for microstructural control.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Measurement of Thermal Conductivity in a Supercooled Hydrogel-Salt Complex Near Its Phase Transition

Solid-liquid phase transitions, i.e. solidification processes, have applications in data storage, development of novel thermoelectric materials, cooling of microelectronic substrates and air conditioning condensers. Standard analyses of solidification (Stefan problem) assume constant thermal properties of the solid and liquid sides. It is not known how these properties change across the spatial transition interface, though most studies report a discontinuity in the solid and liquid properties through the transition temperature [1]. When the phase transition releases enthalpy, recent research has shown if the phonon or electron transport time is of the same order of magnitude as the time scale of the atomic transformation, this increases the heat capacity of the solid material at temperatures near the phase transition temperature [2]. A fundamental understanding of the phase transition may help shed light on the molecular origins of supercooling and spontaneous nucleation, which will help with applications involving them. We report studies of supercooling and nucleation of sodium sulfate decahydrate, a salt hydrate which is of recent interest in thermal storage, and of a hydrogel-sodium sulfate complex which shows limited supercooling. We will also report the measurement of their thermal properties during the phase transition process. This will be done with a hot-wire setup which produces small temperature changes of the order of ~1 C.

crystallization, phase transformation, thermal con↗
DOE OSTI2024

Manuscript Workflows from and Processed Organic Matter Composition of Experimentally Burned Open Air and Muffle Furnace Vegetation Chars across Differing Burn Severity and Feedstock Types from Pacific Northwest, USA (v3)

This dataset includes processed organic matter chemistry data from an experimental study designed to compare how the chemical composition of organic matter changes across different burn conditions and vegetation materials representative of major land cover types of the Pacific Northwest, USA. Chars were created in a closed muffle furnace or on an open burn table from four different feedstock species representing vegetation commonly impacted by fire regimes across the Pacific Northwest, USA. Source data and associated metadata (including methods and geospatial information) can be found at https://data.ess-dive.lbl.gov/datasets/doi:10.15485/1894135 (Grieger et al. 2022). This dataset provides processing scripts and processed data for both solid and dissolved phase organic matter characterization data from experimentally generated chars. These processed data can be used to compare how different burn conditions may influence resultant organic matter chemistry and help further our understanding of potential biogeochemical impacts on river corridors post-fire. The processed data were subsequently analyzed; and the results and ecological implications of the findings were published in peer-reviewed manuscripts. The scripts and workflows used to develop the manuscripts are also included in this data package.This data package was originally published June 2024. It was updated September 2024 (new and modified files) and in January 2025 (modified files). See the change history section in the readme for more details.This dataset is comprised of one data package readme, one data dictionary (dd), one file level metadata (flmd), and folders containing (A) processed data; (B) general processing scripts; and (C) additional folders with specific manuscript analysis scripts and processed data. Step-by-step instructions to assist the user in recreating the workflow used to generate the results in the manuscripts is also provided. The processed data folder includes (1) a folder of processed Parallel Factor Analysis (PARAFAC) and spectra indices outputs from excitation emissions matrix (EEM) fluorescence and absorbance data; (2) a folder of processed solid state carbon-13 (13-C NMR) integrals; (3) folder of high resolution characterization of organic matter via 21 Tesla Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS) generated through the Environmental Molecular Sciences Laboratory (EMSL; https://www.pnnl.gov/environmental-molecular-sciences-laboratory) processed data outputs from Formultitude (https://github.com/PNNL-Comp-Mass-Spec/Formultitude), blank corrections and data aggregation, and calculated molecular indices. All files are .pdf, .csv, .html, .Rmd, .R, or .RData.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

A novel defoamer for processing nuclear waste: Testing and performance

Abstract Legacy radioactive waste from nuclear weapons material processing is the biggest environmental challenge in the state of South Carolina, and one of the biggest in the United States. Although substantial progress has been made in processing and vitrifying high‐level radioactive waste at the Savannah River site, approximately 35 million gallons remains to be treated and dispositioned. In this article, we show the development of a new defoamer for use in the processing of high‐level radioactive waste. The application of the new defoamer is not only more effective at controlling foam but will shorten the batch processing time leading to safer and more efficient processing. This has the potential to help shorten the overall site mission lifetime, saving the federal government hundreds of millions of dollars. The novel aspect of the new defoamer is its effectiveness and stability in the harsh conditions needed for processing high‐level radioactive waste: high temperatures, pH 4–13, strong oxidizing and reducing agents, and numerous metal catalysts. The defoamer will replace an existing antifoam agent that decomposes to form multiple flammable gases. Because the existing antifoam agent decomposes quickly, processing changes increased processing time. Statement of novelty We demonstrate that a new defoamer has been developed for use in processing high‐level radioactive waste. This novel defoamer is effective and stable in the harsh processing conditions with no detectable flammable by‐products. Because the existing antifoam agent decomposes quickly, processing changes, including lowering acid addition rates and evaporation rates, increased processing time. The new defoamer is not only more effective at controlling foam but will shorten the batch processing time and lead to safer and more efficient processing by eliminating the production of flammable gases. Statement of industrial relevance Foaming is of great concern in many industrial processes involving three‐phase gas/liquid/fine‐solids systems, like in water evaporation, mineral floatation, air sparging in situ remediation techniques, and in those found in the paper industry.

Lambert, Dan P.↗
DOE OSTI2018

Modifying High-Voltage Olivine-Type LiMnPO 4 Cathode via Mg Substitution in High-Orientation Crystal

The LiMnPO4 material with Mg2+ ion substitution in transition metal site is successfully obtained by a facile solvothermal method combining with the subsequent spray drying and pyrolysis. The TEM image shows the controlled crystalline orientation of the primary Mg-doped LiMnPO4 particle, and the three-dimensional (3D) hierarchical micronano structure and the electronic structure of the Mg-doped material are investigated by the reconstructed nanotomography and X-ray absorption spectroscopy, respectively. The uniformity of Mg2+ ions substitution at the secondary particle level is confirmed by the transmission X-ray microscopy combined with X-ray absorption near edge structure. The prepared material exhibits an excellent electrochemical performance with the capacity of 156 mAh/g at the rate of 0.1 C, and good capacity retention of 100% after 400 cycles at the rate of 1 C. The in operando synchrotron X-ray diffraction data indicate that the performance improvement of the Mg-doped materials is attributed to the changed electrochemical reaction mechanism from the typical two-phase reaction for pristine LiMnPO4 material to the two-phase reaction combined with the single-phase (solid-solution) reaction process. These findings provide a new approach and understanding on developing high-energy cathode materials for lithium-ion batteries.

high orientation↗
DOE OSTI2026

Modern insights into the mechanisms of neptunium oxalate decomposition

Neptunium oxalate (Np(C 2 O 4 ) 2 ·6H 2 O) is a historically relevant solid phase used in nuclear processing as a precursor for neptunium dioxide (NpO 2 ). Although Np oxalate has been synthesized and used for NpO 2 production for decades, the thermal decomposition mechanism of this phase remains poorly understood and has not been evaluated in over 30 years. Conflicting reports in historical literature suggest either a direct conversion from anhydrous oxalate to NpO 2 or a decomposition that includes the formation of Np carbonate or oxidized Np intermediate phases. In this work, we reexamine the decomposition pathway of Np(C 2 O 4 ) 2 ·6H 2 O using thermal analysis coupled with evolved gas analysis and temperature-dependent Raman spectroscopy to elucidate decomposition mechanisms and intermediate phases using modern analytical techniques. Thermal analysis revealed a three-stage decomposition process, including dehydration below 200 °C, oxalate breakdown between 170 and 370 °C, and NpO 2 formation by 500 °C. However, an unidentified plateau in the thermal data was observed during measurements. Raman spectroscopy confirmed the stages of decomposition, and in the analysis of potential intermediate phases, no carbonate phases or Np 2 O 5 were identified. Raman data suggest that residual oxalate or nonstoichiometric oxide are present during decomposition before pure NpO 2 is formed. These findings clarify aspects of the Np oxalate decomposition mechanism and address longstanding discrepancies in the literature, with a specific focus on Np-specific materials chemistry.

Lawson, Kathryn M. [Oak Ridge National Laboratory ↗
DOE OSTI2020

A practical guide for crystal growth of van der Waals layered materials

This Tutorial provides an overview of the techniques that are most commonly utilized to grow bulk van der Waals crystals. The materials discussed were selected to highlight various challenges that are often encountered during crystal growth. Additionally, in relatively equal parts, the text covers melt-based techniques, vapor transport growths, and the characterization of crystal quality with an emphasis on structural and chemical homogeneities. Furthermore, pertinent details are given regarding the growth and characterization of many specific compounds, with examples mostly drawn from our own research, and an effort is made to highlight cases where the growths offer a particular lesson or the conditions have a significant impact on the crystal’s physical properties. A primary goal is to motivate more researchers to grow crystals by providing general descriptions and considerations for different growth techniques and equipment while sharing some of our own lessons learned and best practices for the growth and characterization of layered van der Waals crystals. The Tutorial is not written solely for aspiring crystal growers, however, because any researcher who collaborates with a crystal grower can benefit from having a greater understanding and appreciation of the processes of crystal growth and materials development.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Destruction of Refractory Carbon in Protoplanetary Disks

The Earth and other rocky bodies in the inner solar system contain significantly less carbon than the primordial materials that seeded their formation. These carbon-poor objects include the parent bodies of primitive meteorites, suggesting that at least one process responsible for solid-phase carbon depletion was active prior to the early stages of planet formation. Potential mechanisms include the erosion of carbonaceous materials by photons or atomic oxygen in the surface layers of the protoplanetary disk. Under photochemically generated favorable conditions, these reactions can deplete the near-surface abundance of carbon grains and polycyclic aromatic hydrocarbons by several orders of magnitude on short timescales relative to the lifetime of the disk out to radii of ∼20–100+ au from the central star depending on the form of refractory carbon present. Due to the reliance of destruction mechanisms on a high influx of photons, the extent of refractory carbon depletion is quite sensitive to the disk’s internal radiation field. Dust transport within the disk is required to affect the composition of the midplane. In our current model of a passive, constant- α disk, where α = 0.01, carbon grains can be turbulently lofted into the destructive surface layers and depleted out to radii of ∼3–10 au for 0.1–1 μ m grains. Smaller grains can be cleared out of the planet-forming region completely. Destruction may be more effective in an actively accreting disk or when considering individual grain trajectories in non-idealized disks.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2021

Process-Structure-Property Relations for As-Deposited Solid-State Additively Manufactured High-Strength Aluminum Alloy

Solid-state additive manufacturing methods provide innovative solutions to circumvent problems associated with materials susceptible to hot cracking by avoiding liquid solid phase transformations. In this work, the process parameter influence on microstructural evolution and mechanical response of a fully dense aluminum alloy 7050 (AA7050) component manufactured via a rapid, solid-state additive manufacturing process known as Additive Friction Stir Deposition (AFS-D) was quantified for the first time. Three sections (starting dwell, transient, crossover of roads) of the deposition that exhibit differing thermomechanical processing histories were evaluated for the resulting microstructure and mechanical response. The microstructural characterization was performed on the as-deposited AA7050 via Electron Backscatter Diffraction (EBSD), TEM, optical microscopy, and Scanning Electron Microscopy (SEM). The microstructural characterization revealed refined constituent particles and grains throughout the as-deposited AA7050 microstructure. Furthermore, quasi-static tensile experiments were conducted in both the build and transverse directions, in order to quantify the orientation influence on tensile properties of the as-deposited AA7050 build. Spatially dependent tensile properties were observed in the material due to heat input variation coarsening of secondary phases towards the initial layers of the AFS-D build. Post-mortem analysis revealed that voids nucleated and coalesced from the overgrowth of the strengthening precipitates present in the material, resulting in fracture.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Optimizing high energy density sulfur cathodes: A multivariate approach to electrode formulation and processing

Lithium-sulfur (Li-S) batteries involve complex solid-liquid-solid phase transformations during both discharging and charging processes, where cathode materials, formulation, and structure play a crucial role. Here, a design of experiments (DoE) methodology and an empirical model are developed to systematically explore the interactions and trade-offs among cathode factors and process variables, and to obtain generalizable effects estimates for the multivariate system. Compared to the conventional one-factor-at-a-time (OFAT) approach, this work demonstrates advantages in both efficiency and accuracy by allowing the data to guide future research and decisions. Further, an optimized cathode formulation and processing parameters are predicted and validated experimentally, achieving over 1000 mAh g -1 in discharge capacity and improved cycling under practical lean electrolyte (4 µL mg -1 S) and high S-loading cathodes (>4 mg cm -2 ) conditions. The optimized cathode was scaled up and assembled into Li-S pouch cells, achieving 316 Wh kg -1 in cell-level energy, proving that the comprehensive and rigorous framework for optimizing complex systems with DoE leads to improved performance in a practical pouch cell system.

25 ENERGY STORAGE↗
DOE OSTI2026

Reduction of Np(v) to Np(iv) using oxalic acid: rethinking decades of nuclear processing conventions

Actinide oxalate precipitation has been ubiquitous in nuclear processing since the 1950s due to its simplicity at laboratory and production scales as both a means of actinide purification and as a key intermediate solid phase towards oxide production. Historical processing information has emphasized the need to reduce actinides, including neptunium (Np), to the tetravalent or trivalent state with chemical reducing agents prior to oxalate precipitation. This work revisits the established method and reveals that oxalic acid has an unexpected role as a reducing agent for Np(v/vi). Also, the study uncovers insights into the direct precipitation of Np(iv) oxalate from neptunyl solutions, as identified by spectroscopic and X-ray diffraction analyses. These findings challenge the long-standing notion that redox adjustment of actinides is necessary for oxalate processing.

Gilson, Sara [ORNL] (ORCID:0009000706842064)↗
DOE OSTI2016

In Situ High Temperature High Pressure MAS NMR Study on the Crystallization of AlPO 4 -5

A damped oscillating crystallization process of AlPO4-5 at the presence of small amount of water is demonstrated by in situ high temperature high pressure multinuclear MAS NMR. Crystalline AlPO4-5 is formed from an intermediate semicrystalline phase via continuous rearrangement of the local structure of amorphous precursor gel. Activated water catalyzes the rearrangement via repeatedly hydrolysis and condensation reaction. Strong interactions between organic template and inorganic species facilitate the ordered rearrangement. During the crystallization process, excess water, phosphate, and aluminums are expelled from the precursor. The oscillating crystallization reflects mass transportation between the solid and liquid phase during the crystallization process. This crystallization process is also applicable to AlPO4-5 crystallized in the presence of a relatively large amount of water.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2024

Simulant Development of Potential 200 West Area Waste Feeds

Preliminary planning for retrieval, qualification, and pretreatment of waste in Hanford’s 200 West Area (200W) has begun as part of the West Area Risk Management project. Experimental studies to technically mature pretreatment process operations will likely be needed because of the uniqueness of 200W waste. Pacific Northwest National Laboratory formulated five simulants to represent 200W-qualified feed based on the preliminary flowsheet provided by Washington River Protection Solutions, LLC. The simulant recipes were devised using applicable historical information as a reference point to support the use of the flowsheet waste vectors, which were combined into five distinct groups. These five groups formed the basis for the liquid composition targets that were adapted into recipes using charged-balanced salt species. The liquid phase recipes were batched in 1-L quantities and analyzed at Pacific Northwest National Laboratory. Once confirmed to be stable, the liquid solutions were tested for compatibility with candidate solid components. Specific solid components were recommended based on cross-examining the proposed solid phases in the flowsheet with relevant data from the literature. Mixtures of solid components were added to aliquots of the liquid batches and sub-sampled to measure particle size distribution. The measured distribution was compared to independently created benchmark distributions appropriate for each simulant. This process was iterated until a solid phase composition that resulted in a representative particle size distribution was found. After the final compositions were confirmed, a suite of chemical and physical characterization data was collected. This report describes the simulant basis, formulation methodology, laboratory measurements, and data collected for the recipes recommended to represent 200W waste feeds.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2022

An improved process for the release of synthetic DNA sequences from a solid-phase capture support

Here, to facilitate the solid-phase purification of synthetic DNA sequences, a riboside phosphoramidite, carrying a 5-O-capture linker and a 2-O-silyl ether protecting group, is incorporated into a DNA sequence during its last solid-phase synthesis cycle. After deprotection and release of the DNA sequence from the synthesis support, the sequence is then covalently linked to a capture support to enable the removal of shorter unbound DNA sequences by simply washing these off the support. The solid-phase purified DNA sequence is then released from the capture support, through an innovative intramolecular cyclodeesterification of its terminal riboside ethyl phosphate triester entity and is isolated in a yield of 94% while displaying an exquisite purity of 97%.

59 BASIC BIOLOGICAL SCIENCES↗