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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 775 records · Page 43
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Effect of overcharge on Li(Ni 0.5 Mn 0.3 Co 0.2 )O 2 /graphite lithium ion cells with poly(vinylidene fluoride) binder. III — Chemical changes in the cathode

Here, 1.5 Ah pouch cells based on Li(Ni 0.5 Mn 0.3 Co 0.2 )O 2 cathodes and graphite anodes, both containing poly (vinylidene fluoride) (PVDF) binders, were systematically overcharged to 100, 120, 140, 160, 180, and 250% state of charge (SOC), at which point they vented. The cells were subsequently discharged to 0% SOC and disassembled under an inert atmosphere for characterization. A combination of X-ray photoelectron spectroscopy (XPS), scanning-electron microscopy (SEM), energy-dispersive spectroscopy (EDS), 6 Li SSNMR, and X-ray diffraction (XRD) analysis of the NMC532 cathodes indicates the formation of a thin C- and O-rich cathode electrolyte interphase layer, progressive Li loss above 140% SOC, and retention of the bulk crystal structure at all states of charge.

25 ENERGY STORAGE↗
DOE OSTI2020

Bulk vs Intrinsic Activity of NiFeO x Electrocatalysts in the Oxygen Evolution Reaction: The Influence of Catalyst Loading, Morphology, and Support Material

We used a combination of ultrahigh vacuum surface science techniques, X-ray spectroscopy, electrochemistry, and density functional theory (DFT), to characterize the influence of catalyst morphology, loading/coverage, and substrate material on the bulk (all atoms) and intrinsic (electrochemically accessible atoms) activity of NiFeO x electrocatalysts in the oxygen evolution reaction (OER). NiFeO x catalysts were grown on both Au(111) and highly oriented pyrolytic graphite (HOPG) electrodes. DFT predicted Fe edge-site atoms at the NiFeO x /Au(111) interface to be the most thermodynamically favorable reaction center, and X-ray absorption spectroscopy data indicated small NiFeO x catalyst particles on Au(111) contained a high population of OER active Fe edge-site atoms. However, restructuring of the Au(111) surface due to repeated oxidation and reduction cycles of the OER CV measurements encapsulated small NiFeO x nanoparticles at catalyst loadings below ~1.5 nmol metal /cm 2 , passivated catalyst edges and reduced bulk OER activity of Au-supported NiFeO x compared with HOPG-supported ones. Analysis of intrinsic activity revealed that the Au(111) support strongly benefited electrochemically accessible NiFeO x atoms, and we observed a 2–3 fold activity enhancement compared with HOPG-supported catalysts for loadings above ~1 nmol metal /cm 2 . Overall, evaluating bulk vs intrinsic activity and identifying loading/coverage-dependent support effects is important for accurately probing fundamental interfacial chemistry, choosing suitable catalyst loadings and supports, and optimizing system parameters to maximize the performance of electrocatalyst systems.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Casting and Characterization of U-50Zr

Uranium alloyed with 50 wt% zirconium (U-50Zr) is a proposed light water reactor (LWR) nuclear fuel by Lightbridge Corporation (LTBR). The proposed method for making the U-50Zr alloy is to arc-melt master alloys and then remelt in a vacuum induction melter (VIM) to consolidate the material and cast into an intermediate shape. After casting, the material will eventually need to be formed into a desired fuel shape. The work discussed in this report resulted from a joint effort between Ltbr and Pacific Northwest National Laboratory (PNN) to investigate a 500g – 1kg scale casting process to produce the U-50Zr alloy in the desired δ-UZr 2 phase and characterize the impurities and microstructure that result from the casting process. Master alloys were fabricated in an arc melter, then five castings were carried out in a VIM with multiple inert coating and crucible materials to find an appropriate combination. Both ZrO 2 and graphite crucibles were used and different combinations of Y 2 O 3 , CaZrO 3 , and TiC to identify which would contain the molten metal with the least reaction. On each casting, the C, O, N, H impurities were analyzed as well as the phase by x-ray diffraction and microstructure. Of the five castings, two resulted in majority of δ-UZr 2 phase-pure material and had impurity levels within acceptable ranges. The two most successful castings utilized a graphite crucible with a TiC undercoating and a Y 2 O 3 overcoat. The O and N levels were below 1000 ppm and the C content was variable but did not result in measurable carbide formation. The highest success casting resulted in an average of 282 ppm C, 567 ppm O, 217 ppm N and 79 ppm H. This casting's crucible and inert coating material was repeated with slightly different casting parameters and resulted in higher C numbers but similar phase identification. The differences between each casting are discussed and recommendations are made for future experiments to better decide on a casting process to go forward with.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS2018

Development of Large Bandgap Materials Using Reactive Growth in Al-SI Eutectic for Optical and RF Applications

Carbon was utilized as reactive element to modify the microstructure using forced mixing during crystallization of the Al-Si alloy by rotation and stirring. We nucleated the material on SiC substrates while the Al-Si melt was rotated with a speed of 30rpm in a graphite crucible. Several experiments were performed and parameters such as time of mixing, soaking temperature, rotation rate of the substrate and rate of cooling during the solidification was changed. We observed dendrite and cell morphologies during the solidification of rotating melt. The microstructure was characterized by optical microscopy and SEM-EDX and compositional spectroscopy. The effect of carbon impurities was studied on the solidifying microstructure. When we used the longer soak time of the melt in presence of carbon impurities we observed the destruction of dendritic morphology and the formation of cellular and colony structures. Similar approach has been used for Ga2O3, a novel large bandgap material also.

Singh, N. B.↗
NASA NTRS2006

History of Metal Veins in Acapulcoite-Lodranite Clan Meteorite GRA 95209

Graves Nunataks (GRA) 95209 has been hailed as the missing link of core formation processes in the acapulcoitelodranite parent asteroid because of the presence of a complex cm-scale metal vein network. Because the apparent liquid temperature of the metal vein (approximately 1500 C) is higher than inferred for the metamorphic grade of the meteorite, questions regarding the vein s original composition, temperature, and mechanism of emplacement have arisen. We have determined trace siderophile element compositions of metals in veins and surrounding matrix in an effort to clarify matters. We analyzed metals in GRA 95209 in a portion of thick metal vein and adjacent metal-rich (30-40 modal%), sulfide poor (less than 1%) matrix by EPMA and LA-ICP-MS for major and trace siderophile elements using methods described by [3]. We also examined metals from a metal-poor (approximately 15 modal%) and relatively sulfide-rich (2-5 modal%) region of the sample. Kamacite is the dominant metal phase in all portions of the sample. In comparison to matrix metal, vein metal contains more schreibersite and less tetrataenite, and is less commonly associated with Fe,Mn,Mg-bearing phosphates and graphite. Vein kamacite contains higher Co, P, and Cr and lower Cu and Ge. These minor variations aside, all metal types in GRA 95209 are fairly homogeneous in terms of their levels of enrichment of compatible siderophile elements (e.g. Pt, Ir, Os) relative to incompatible siderophile elements (e.g. As, Pd, Au), consistent with the loss of metal-sulfide partial melt that characterizes much of the clan. Whatever compositional differences between matrix and vein metal that may have originally existed, they have since largely co-equilibrated to similar restitic trace element compositions. We agree with [2] that metal veins, in their present state, do not represent a liquid composition. The original vein liquid was much more S-rich and emplaced at correspondingly lower liquid temperatures. Much of the Fe,Ni component solidified in cm scale conduits while S-rich melts were expelled and continued to migrate by percolation. The higher troilite content in metal poor regions of the sample results mostly from trapping of a small portion of these melts. The troilite is not remnant primary sulfide. Strong depletions of W, Mo, and especially Ga (greater than 50%, greater than 60%, and greater than 90% depletion, respectively) in metals of the metalpoor GRA 95209 lithology are localized at scales of 10-100 micrometers in the vicinity of graphite spherules. These depletions must have occurred below the temperatures at which cm-scale equilibration occurred, and future work will seek to determine their cause.

Herrin, J. S.↗
DOE OSTI2021

Encapsulation of metal nanoparticles at the surface of a prototypical layered material

Encapsulation of metal nanoparticles just below the surface of a prototypical layered material, graphite, is a recently discovered phenomenon. These encapsulation architectures have potential for tuning the properties of two-dimensional or layered materials, and additional applications might exploit the properties of the encapsulated metal nanoclusters themselves. The encapsulation process produces novel surface nanostructures and can be achieved for a variety of metals. Because these studies of near-surface intercalation are in their infancy, these systems provide a rich area for future studies. This Review presents the current progress on the encapsulation, including experimental strategies and characterization, as well as theoretical understanding which leads to the development of predictive capability. The Review closes with future opportunities where further understanding of the encapsulation is desired to exploit its applications.

encapsulation↗
DOE OSTI2013

Blackbody comparator for thermocouple calibration

MIKES is developing a measurement set-up for calibrating thermocouples in the temperature range 960 °C - 1500 °C. The calibration method is based on direct comparison of thermocouples and radiation thermometers. We have designed a graphite blackbody comparator cell, which is operated in a horizontal single-zone tube furnace. The cell includes two blackbody cavities for radiation temperature measurements. The cavities have openings on opposite sides of the cell, allowing simultaneous measurement with two radiation thermometers. The design of the comparator allows three thermocouples to be calibrated simultaneously. The thermocouples to be calibrated are inserted in thermometer wells around one of the measurement cavities. We characterize the blackbody comparator in terms of repeatability, temperature distribution and emissivity. Finally, we validate the uncertainty analysis by comparing calibration results obtained for type B and S thermocouples to the calibration results reported by Technical Research Institute of Sweden (SP), and MIKES. The agreement in the temperature range 1000 °C - 1500 °C is within 0.90 °C, the average deviation being 0.17 °C.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2025

Neutron-Friendly Li-Ion Battery Coin Cell for In Situ 3D Visualization of Li Plating

Advanced battery characterization using in situ/operando neutron imaging is critical for uncovering degradation modes such as lithium (Li) plating in Li-ion batteries (LIBs). However, conventional LIBs hinder operando neutron radiography (NR) and in situ neutron micro-computed tomography (N-μCT) for visualizing Li plating near the graphite-separator interface due to strong attenuation from hydrogen-rich components like PP–PE–PP separators, electrolyte, and Fe-based spacers. In this work, we designed and tested a neutron-friendly battery (NFB) optimized for in situ Li detection during extreme fast charging (XFC). Guided by neutron attenuation cross-sections and material transmission, the NFB enables clear visualization at the graphite–separator interface, which is typically opaque in standard LIBs. Electrochemical tests show the NFB exhibits voltage/current responses like standard cells for up to 50 XFC cycles. However, its lower reversibility and capacity are likely due to Cu-coated Al spacer degradation from delamination or corrosion. We propose titanium spacers as a more stable alternative, albeit requiring custom machining. Using this optimized cell, we achieved simultaneous neutron tomography of multiple cells, capturing in situ 3D images of dead Li accumulation, particularly near graphite edges. These heterogeneous deposits and disconnected Li clusters suggest localized current density hotspots during XFC.

25 ENERGY STORAGE↗
DOE OSTI2023

Irreparable Interphase Chemistry Degradation Induced by Temperature Pulse in Lithium–Ion Batteries

While it is widely recognized that the operating temperature significantly affects the energy density and cycle life of lithium-ion batteries, the consequence of electrode-electrolyte interphase chemistry to sudden environmental temperature changes remains inadequately understood. Here, we systematically investigate the effects of a temperature pulse (T pulse) on the electrochemical performance of LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) pouch full cells. By utilizing advanced characterization tools, such as time-of-flight secondary-ion mass spectrometry, we reveal that the T pulse can lead to an irreversible degradation of cathode-electrolyte interphase chemistry and architecture. Despite negligible immediate impacts on the solid-electrolyte interphase (SEI) on graphite anode, aggregated cathode-to-anode chemical crossover gradually degrades the SEI by catalyzing electrolyte reduction decomposition and inducing metallic dead Li formation because of insufficient cathode passivation after the T pulse. Consequently, pouch cells subjected to the T pulse show an inferior cycle stability to those free of the T pulse. Furthermore, this work unveils the effects of sudden temperature changes on the interphase chemistry and cell performance, emphasizing the importance of a proper temperature management in assessing performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Human Airway Epithelial Cell Responses to Single Walled Carbon Nanotube Exposure: Nanorope-Residual Body Formation

This investigation examines the 'first contact responses' of in vitro human epithelial airway cells exposed to unrefined single walled carbon nanotubes (SWCNTs) [containing metal catalyst, carbon black, amorphous carbon, graphitic shells, and SWCNTs], and refined acid/peroxide cleaned and cut SWCNTs at low and high dose exposures (0.16 ug/L and 1.60 ug/L) for 2, 3 and 3.5 hours. FTIR, X-ray compositional analysis, morphological TEM analysis and UV-Vis were used to physicochemically characterize the SWCNTs in this study. Following SWCNT exposure to human lung NCI-H292 epithelial monolayers, the airway cells were prepared for light microscopy vital staining, or fixed in glutaraldehyde for SEM/TEM imaging to determine SWCNT binding, uptake, intracellular processing and organellar/SWCNT fate within the exposure period. At 2 hr exposures to both unrefined Carbolex, and refined SWCNTs (at both high and low doses), there were no increases in lung cell necrosis compared to controls. However high dose, 3 hr exposures to unrefined Carbolex material produced severe cell damage (apical and basal plasma membrane holes, decreased mitochondria, numerous intracellular vesicles containing nanomaterial and membrane fragments) and increased cell necrosis. The refined SWCNTs exposed for 3 hr at low dose produced no increase in cell death, although high dose exposure produced significant cell death. By TEM, Acid/peroxide cleaned SWCNT 3 hr exposures at high and low doses, revealed SWCNTs attachment to cell surface mucin, and SWCNT uptake into the cells during membrane recycling. Membranes and SWCNTs were seen within cytoplasmic lamellar body-type vesicles, where vesicular contents were bio-degraded, eventually forming long SWCNT-nanoropes, which were subsequently released into the cytoplasm as clusters of attached nanoropes, as the vesicle membranes fragmented. These Nanorope-Residual Bodies did not cause damage to the surrounding organelles or cytoplasm, and seemed very stabile in the cell cytoplasm. To our knowledge this is the first time that human lung cells have been shown to very rapidly bind, incorporate, bio-degrade and re-assemble SWCNTs into nanoropes intracellularly, to form stabile Nanorope Residual bodies.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
NASA NTRS1976

Chemical fractionations in meteorites. X - Ureilites

An investigation involving the measurement of 17 trace elements in 4 ureilites was conducted with the objective to obtain information for the characterization of the two components of the ureilites. The groundmass of the mineral is an olivine-clinopyroxene rock which is presumably the residue left after partial melting of a more primitive precursor. This ultramafic rock is permeated by a network of veins containing diamond, graphite, nickel-iron, and primordial noble gases. Attention is given to the vein material, the origin of the vein material, the 'constant' siderophile component and ultramafic rock, and questions concerning the origin of ureilites.

Higuchi, H.↗
NASA NTRS1988

Status of Gr/glass composites technology at UTOS

The TSC (Thermally Stable Composite) refers to a family of graphite reinforced glass matrix composite materials developed by UTOS. This fiber matrix combination exhibits low coefficients of thermal expansion (CTE), exceptional dimensional stability, high specific strength and stiffness, adequate fracture toughness, and space environment compatibility. The dimensional stability of a TSC mirror structure was experimentally characterized at the Steward Observatory. Preliminary results indicate that TSC is significantly more thermally stable than most current structural composite materials. In addition, the use of lower CTE glass matrix materials, such as 96 percent silica glass, have the potential for producing graphite/glass panels with expansion rates and stability comparable to that of fused silica.

Mayor, Ramon A.↗
DOE OSTI2014

Origin of graphitic filaments on improving the electron field emission properties of negative bias-enhanced grown ultrananocrystalline diamond films in CH{sub 4}/Ar plasma

Microstructural evolution of bias-enhanced grown (BEG) ultrananocrystalline diamond (UNCD) films has been investigated using microwave plasma enhanced chemical vapor deposition in gas mixtures of CH{sub 4} and Ar under different negative bias voltages ranging from −50 to −200 V. Scanning electron microscopy and Raman spectroscopy were used to characterize the morphology, growth rate, and chemical bonding of the synthesized films. Transmission electron microscopic investigation reveals that the application of bias voltage induced the formation of the nanographitic filaments in the grain boundaries of the films, in addition to the reduction of the size of diamond grains to ultra-nanosized granular structured grains. For BEG-UNCD films under −200 V, the electron field emission (EFE) process can be turned on at a field as small as 4.08 V/μm, attaining a EFE current density as large as 3.19 mA/cm{sup 2} at an applied field of 8.64 V/μm. But the films grown without bias (0 V) have mostly amorphous carbon phases in the grain boundaries, possessing poorer EFE than those of the films grown using bias. Consequently, the induction of nanographitic filaments in grain boundaries of UNCD films grown in CH{sub 4}/Ar plasma due to large applied bias voltage of −200 V is the prime factor, which possibly forms interconnected paths for facilitating the transport of electrons that markedly enhance the EFE properties.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Enhanced charge separation ability and visible light photocatalytic performance of graphitic carbon nitride by binary S, B co-doping

Highlights: • S, B hertroatoms were successfully doped into g-C{sub 3}N{sub 4} by thermal treatment. • S, B heteroatoms effectively change the intrinsic electronic structure of g-C{sub 3}N{sub 4}. • The SBCN shows much higher photocatalytic activity than CN, SCN and BCN. • The SBCN has high photocatalytic stability and reusability. - Abstract: As a metal-free visible light photocatalyst, the photocatalytic performance of graphitic carbon nitride (g-C{sub 3}N{sub 4}) is limited. To improve the activity of g-C{sub 3}N{sub 4}, we herein report a binary S, B co-doped g-C{sub 3}N{sub 4} (SBCN) by thermally treating the precursor mixture of thiourea, melamine and boron oxide. Characterization results show the obtained SBCN has ultrathin sheet-like morphology and these doped heteroatoms are uniform distributed in the sample. Compared to the pristine g-C{sub 3}N{sub 4}, the SBCN has a small band gap with additional absorption in visible light region, decreased photoluminescence emission and electric resistance and enhanced photocurrent response. These advantages endue SBCN with excellent photocatalytic activity for degradation of organic dyes, and its reaction rate is 6.5 times higher than that of the g-C{sub 3}N{sub 4}. Moreover, the successive cycles demonstrate that this SBCN possesses a superior stability and reusability. Finally, we propose a possible photocatalytic mechanism based on the band structure and mainly active species.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

The structure of PccH from Geobactersulfurreducens-a novel low reduction potential monoheme cytochrome essential for accepting electrons from an electrode

The structure of cytochrome c (GSU3274) designated as PccH from Geobactersulfurreducens was determined at a resolution of 2.0 angstrom. PccH is a small (15kDa) cytochrome containing one c-type heme, found to be essential for the growth of G.sulfurreducens with respect to accepting electrons from graphite electrodes poised at -300mV versus standard hydrogen electrode. with fumarate as the terminal electron acceptor. The structure of PccH is unique among the monoheme cytochromes described to date. The structural fold of PccH can be described as forming two lobes with the heme sandwiched in a cleft between the two lobes. In addition, PccH has a low reduction potential of -24mV at pH7, which is unusual for monoheme cytochromes. Based on difference in structure, together with sequence phylogenetic analysis, we propose that PccH can be regarded as a first characterized example of a new subclass of class I monoheme cytochromes. The low reduction potential of PccH may enable the protein to be redox active at the typically negative potential ranges encountered by G. sulfurreducens. Because PccH is predicted to be located in the periplasm of this bacterium, it could not be involved in the first step of accepting electrons from the electrode but is very likely involved in the downstream electron transport events in the periplasm.

Dantas, Joana↗
DOE OSTI2021

Electrochemical ion insertion from the atomic to the device scale

Electrochemical ion insertion involves coupled ion–electron transfer reactions, transport of guest species and redox of the host. The hosts are typically anisotropic solids with 2D conduction planes but can also be materials with 1D or isotropic transport pathways. These insertion compounds have traditionally been studied in the context of energy storage but also find extensive applications in electrocatalysis, optoelectronics and computing. Recent developments in operando, ultrafast and high-resolution characterization methods, as well as accurate theoretical simulation methods, have led to a renaissance in the understanding of ion-insertion compounds. In this Review, we present a unified framework for understanding insertion compounds across timescales and length scales ranging from atomic to device levels. Using graphite, transition metal dichalcogenides, layered oxides, oxyhydroxides and olivines as examples, we explore commonalities in these materials in terms of point defects, interfacial reactions and phase transformations. We illustrate similarities in the operating principles of various ion-insertion devices, ranging from batteries and electrocatalysts to electrochromics and thermal transistors, with the goal of unifying research across disciplinary boundaries.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Characterization of laser-induced plasmas as a complement to high-explosive large-scale detonations

Experimental investigations into the characteristics of laser-induced plasmas indicate that LIBS provides a relatively inexpensive and easily replicable laboratory technique to isolate and measure reactions germane to understanding aspects of high-explosive detonations under controlled conditions. Furthermore, we examine spectral signatures and derived physical parameters following laser ablation of aluminum, graphite and laser-sparked air as they relate to those observed following detonation of high explosives and as they relate to shocked air. Laser-induced breakdown spectroscopy (LIBS) reliably correlates reactions involving atomic Al and aluminum monoxide (AlO) with respect to both emission spectra and temperatures, as compared to small- and large-scale high-explosive detonations. Atomic Al and AlO resulting from laser ablation and a cited small-scale study, decay within ~10 -5 s, roughly 100 times faster than the Al and AlO decay rates (~10 -3 s) observed following the large-scale detonation of an Al-encased explosive. Temperatures and species produced in laser-sparked air are compared to those produced with laser ablated graphite in air. With graphite present, CN is dominant relative to N 2 + . Thus, in studies where the height of the ablating laser's focus was altered relative to the surface of the graphite substrate, CN concentration was found to decrease with laser focus below the graphite surface, indicating that laser intensity is a critical factor in the production of CN, via reactive nitrogen.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
NASA NTRS1992

Delamination behavior of quasi-isotropic graphite epoxy laminates subjected to tension and torsion loads

Sixteen and thirty-two ply quasi-isotropic laminates fabricated from AS4/3501-6 were subjected to pure tension, simultaneous tension and torsion, and torsion fatigue. Layups tested were (45 sub n/-45 sub n/O sub n/90 sub n) sub s, with n = 2 or 4. A torsion damage pattern consisting of a localized matrix crack and delaminations was characterized, and the measured torsional stiffnesses were compared with calculated values. It was found that a combination of tension and torsion led to failure at smaller loads than either type of deformation acting alone. Further work is required to determine the exact form of the failure criterion.

Hinkley, J. A.↗