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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 847 records · Page 47
All sourcesNASA NTRSDOE OSTI
DOE OSTI2013

Surface phenomena during the early stages of sintering in steels modified with Fe–Mn–Si–C master alloys

The characteristics of the metallic powder surface play a critical role in the development of strong bonds between particles during sintering, especially when introducing elements with a high affinity for oxygen. In this study, Mn and Si have been combined in a Fe–Mn–Si–C master alloy powder in order to reduce their chemical activity and prevent oxidation during the heating stage of the sintering process. However, when this master alloy powder is mixed with an iron base powder, differences in chemical activity between both components can lead to an oxygen transfer from the iron base powder to the surface of the master alloy particles. The present research is focused on studying the evolution of the master alloy particle surface during the early stages of sintering. Surface characterization by X-ray Photoelectron Spectroscopy (XPS) shows that the master alloy powder surface is mostly covered by a thin easily reducible iron oxide layer (∼ 1 nm). Mn–Si particulate oxides are found as inclusions in specific areas of the surface. Evolution of oxides during sintering was studied on green compacts containing iron powder, graphite and Fe–Mn–Si–C master alloy powder that were heat treated in vacuum (10{sup −6} mbar) at different temperatures (from 400, 600, 800 to 1000 °C) and analyzed by means of XPS. Vacuum sintering provides the necessary conditions to remove manganese and silicon oxides from the powder surface in the range of temperatures between 600 °C and 1000 °C. When sintering in vacuum, since the gaseous products from reduction processes are continuously eliminated, oxidation of master alloy particles due to oxygen transfer through the atmosphere is minimized. - Highlights: • Mn and Si were introduced in sintered steels using a master alloy powder. • Surface of the master alloy is mainly covered by an easily reducible iron oxide. • Temperature ranges for oxidation/reduction are identified. • Vacuum conditions avoid oxygen transfer to oxidation sensitive elements. • Chemical activity of Mn and Si is lowered when combined in a form of master alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Decomposition of W(CO)[subscript 6] at high pressures and temperatures

The decomposition of hexacarbonyltungsten, W(CO){sub 6}, has been studied. The decomposition was induced by heating W(CO){sub 6} in an autoclave at 523 K and pressures up to 1.8 MPa, and by laser heating in a diamond anvil cell at pressures between 5 and 18 GPa. The products have been characterized using synchrotron X-ray diffraction, pair distribution function analysis, Raman spectroscopy and scanning electron microscopy. Decomposition in the autoclave at the lower pressures resulted in the formation of a metastable tungsten carbide, W{sub 2}C, with an average particle size of 1-2 nm, and an unidentified nanocrystalline tungsten oxide and nanocrystalline graphite with average particle sizes of 1-2 and 11 nm, respectively. The existence of nanocrystalline graphite was deduced from micro-Raman spectra and the graphite particle size was extracted from the intensities of the Raman modes. The high-pressure decomposition products obtained in the diamond anvil cell are the monoclinic tungsten oxide phase WO{sub 2} and the high-pressure phase W{sub 3}O{sub 8}(I). The approximate average size of the graphite particles formed here was 6-8 nm. The bulk modulus of W(CO){sub 6} is B{sub 0} {approx_equal} 13 GPa.

36 MATERIALS SCIENCE↗
NASA NTRS2002

Structural Response of Compression-Loaded, Tow-Placed, Variable Stiffness Panels

Results of an analytical and experimental study to characterize the structural response of two compression-loaded variable stiffness composite panels are presented and discussed. These variable stiffness panels are advanced composite structures, in which tows are laid down along precise curvilinear paths within each ply and the fiber orientation angle varies continuously throughout each ply. The panels are manufactured from AS4/977-3 graphite-epoxy pre-preg material using an advanced tow placement system. Both variable stiffness panels have the same layup, but one panel has overlapping tow bands and the other panel has a constant-thickness laminate. A baseline cross-ply panel is also analyzed and tested for comparative purposes. Tests performed on the variable stiffness panels show a linear prebuckling load-deflection response, followed by a nonlinear response to failure at loads between 4 and 53 percent greater than the baseline panel failure load. The structural response of the variable stiffness panels is also evaluated using finite element analyses. Nonlinear analyses of the variable stiffness panels are performed which include mechanical and thermal prestresses. Results from analyses that include thermal prestress conditions correlate well with measured variable stiffness panel results. The predicted response of the baseline panel also correlates well with measured results.

Wu, K. Chauncey↗
NASA NTRS2001

Purification Procedures for Single-Wall Carbon Nanotubes

This report summarizes the comparison of a variety of procedures used to purify carbon nanotubes. Carbon nanotube material is produced by the arc process and laser oven process. Most of the procedures are tested using laser-grown, single-wall nanotube (SWNT) material. The material is characterized at each step of the purification procedures by using different techniques including scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM), Raman, X-ray diffractometry (XRD), thermogravimetric analysis (TGA), nuclear magnetic resonance (NMR), and high-performance liquid chromatography (HPLC). The identified impurities are amorphous and graphitic carbon, catalyst particle aggregates, fullerenes, and hydrocarbons. Solvent extraction and low-temperature annealing are used to reduce the amount of volatile hydrocarbons and dissolve fullerenes. Metal catalysts and amorphous as well as graphitic carbon are oxidized by reflux in acids including HCl, HNO3 and HF and other oxidizers such as H2O2. High-temperature annealing in vacuum and in inert atmosphere helps to improve the quality of SWNTs by increasing crystallinity and reducing intercalation.

Gorelik, Olga P.↗
DOE OSTI2020

Investigating the Effects of Lithium Deposition on the Abuse Response of Lithium-Ion Batteries

Li deposition at the graphitic anode is widely reported in literature as one of the leading causes of capacity fade in lithium-ion batteries (LIBs). Previous literature has linked Li deposition resulting from low-temperature ageing to diminished safety characteristics, however no current research has probed the effects of Li deposition on the abuse response of well-characterized cells. Using overtemperature testing, a relationship between increased concentrations of Li deposition and exacerbated abuse response in 1 Ah pouch cells has been established. A novel Li deposition technique is also investigated, where cells with n:p < 1 (anode-limiting) have been cycled at a high rate to exploit Li + diffusion limitations at the anode. Scanning Electron Microscopy of harvested anodes indicates substantial Li deposition in low n:p cells after 20 cycles, with intricate networks of Li(s) deposits which hinder Li + intercalation/deintercalation. Peak broadening and decreased amplitude of differential capacity plots further validates a loss of lithium inventory to Li + dissolution, and Powder X-ray Diffraction indicates Li + intercalation with staging in anode interstitial sites as the extent of Li deposition increases. A cradle-to-grave approach is leveraged on cell fabrication and testing to eliminate uncertainty involving the effects of cell additives on Li deposition and other degradation mechanisms.

25 ENERGY STORAGE↗
DOE OSTI2017

Design and Demonstration of Three-Electrode Pouch Cells for Lithium-Ion Batteries

Simple three-electrode pouch cells which can be used in distinguishing the voltage and resistance in individual electrodes of lithium ion batteries have been designed. Baseline (1 mm-staggered alignment, cathode away from a reference electrode) and aligned electrodes to a reference electrode located outside of the anode and cathode were studied to see alignment effects on resistance analysis. Cells composed of A12 graphite anodes, LiNi 0.5 Mn 0.3 Co 0.2 O 2 (NMC 532 or NCM 523) cathodes, lithium foil references, microporous tri-layer membranes, and electrolytes, were cycled with cathode cutoff voltages between 3.0 V and 4.3 V for formation cycles or 4.6 V for C-rate performance testing. By applying a hybrid pulse power characterization (HPPC) technique to the cells, resistances of the baseline cells contributed by the anode and cathode were found to be different from those of the aligned cells, although overall resistances were close to ones from aligned cells. As a result, resistances obtained via electrochemical impedance spectroscopy (EIS) and 2D simulation were also compared with those obtained from HPPC.

25 ENERGY STORAGE↗
DOE OSTI2016

Carbon Composite Microelectromechanical Systems (CMEMS)

Pyrolyzed carbon as a mechanical material is promising for applications in harsh environments. In this work, we characterized the material and developed novel processes for fabricating carbon composite micro-electromechanical systems (CMEMS) structures. A novel method of increasing Young's modulus and the conductivity of pyrolyzed AZ 4330 was demonstrated by loading the films with graphene oxide prior to pyrolysis. By incorporating 2 wt.% graphene stiffeners into the film, a 65% increase in Young's modulus and 11% increase in conductivity were achieved. By reactive ion etching pyrolyzed blanket AZ 50XT thick film photoresist, a high aspect ratio process was demonstrated with films >7.5um thick. Two novel multi-level, volume-scalable CMEMS processes were developed on 6" diameter wafers. Young's modulus of 23 GPa was extracted from nanoindentation measurements of pyrolyzed AZ 50XT films. The temperature-dependent resistance was characterized from room temperature to 500C and found to be nearly linear over this range. By fitting the results of self-heated bridges in an inert ambient, we calculated that the bridges survived to 1000C without failure. Transmission electron microscopy (TEM) results showed the film to be largely amorphous, containing some sub-micrometer sized graphite crystallites. This was consistent with our Raman analysis, which also showed the film to be largely sp 2 bonded. The calculated average density of pyrolyzed AZ 4330 films was 1.32 g/cm 2 . Thin level of disorder and the conductivity of thin film resistors were found to unchanged by 2Mrad gamma irradiation from a Co 60 source. Thin film pyrolyzed carbon resistors were hermetically sealed in a nitrogen ambient in 24-pin dual in-line packages (DIP's). The resistance was measured periodically and remained constant over 6 months' time.

36 MATERIALS SCIENCE↗
NASA NTRS1984

Structural Characterization of Solar Silicon

Compared to single crystal silicon, solar silicon generally contains large residual stresses and numerous structural defects. During subsequent processing, the defect structure can undergo further changes since, at the high temperatures required for diffusion, dislocations are sufficiently mobile to rearrange themselves in patterns which reduce long range residual stresses. This process, which is similar to the polygonization of strained metals, has no counterpart in single crystal silicon. Many of the solar silicon materials are grown from graphite dies and crucibles and therefore contain carbon concentrations in excess of 1E18. The interactions between carbon, crystal defects, intrinsic point defects, oxygen and diffusing dopants are discussed.

Ast, D. G.↗
DOE OSTI2015

A covariance methodology for theoretically generated thermal neutron inelastic scattering data - 14502

The The S(α,β) double-differential thermal neutron scattering law tabulated in ENDF File 7 is, by convention, produced theoretically through fundamental scattering physics models for material-specific interatomic structures. Differential and integral inelastic scattering cross sections are calculated by numerically integrating over S(α,β). This information is supplied to nuclear system simulation codes. For systems with a significant thermal neutron flux, calculated system response parameters can be sensitive to this thermal cross section data. Formats and procedures are currently established for representing uncertainty information, or covariances, for various types of ENDF reaction data. However, no published ENDF evaluations contain covariance data for S(α,β) or associated differential and integral inelastic scattering cross sections. Furthermore, no accepted methodology exists for quantifying or representing covariances for this thermal scattering data. For most solids, the influence of a material's interatomic structure and dynamics on inelastic scattering cross sections can be adequately described through the phonon density of states (DOS). The phonon DOS is a probability density function of the population of available vibrational modes in energy, and it is typically the fundamental input for calculating S(α,β). Probable variation in the spectral shape of the phonon DOS may be established which characterizes uncertainties in the physics models and methodology employed in its production. Through Monte Carlo sampling of perturbations from the reference phonon spectrum, an S(α,β) covariance matrix may be generated. With appropriate sensitivity information, this can be propagated to generate covariance data for differential and integral inelastic scattering cross sections. In this work, hexagonal graphite is used as an example material for the purpose of demonstrating procedures for analyzing, calculating and representing uncertainty information for thermal neutron inelastic scattering data. (authors)

42 ENGINEERING↗
NASA NTRS2003

Quantitating Iron in Serum Ferritin by Use of ICP-MS

A laboratory method has been devised to enable measurement of the concentration of iron bound in ferritin from small samples of blood (serum). Derived partly from a prior method that depends on large samples of blood, this method involves the use of an inductively-coupled-plasma mass spectrometer (ICP-MS). Ferritin is a complex of iron with the protein apoferritin. Heretofore, measurements of the concentration of serum ferritin (as distinguished from direct measurements of the concentration of iron in serum ferritin) have been used to assess iron stores in humans. Low levels of serum ferritin could indicate the first stage of iron depletion. High levels of serum ferritin could indicate high levels of iron (for example, in connection with hereditary hemochromatosis an iron-overload illness that is characterized by progressive organ damage and can be fatal). However, the picture is complicated: A high level of serum ferritin could also indicate stress and/or inflammation instead of (or in addition to) iron overload, and low serum iron concentration could indicate inflammation rather than iron deficiency. Only when concentrations of both serum iron and serum ferritin increase and decrease together can the patient s iron status be assessed accurately. Hence, in enabling accurate measurement of the iron content of serum ferritin, the present method can improve the diagnosis of the patient s iron status. The prior method of measuring the concentration of iron involves the use of an atomic-absorption spectrophotometer with a graphite furnace. The present method incorporates a modified version of the sample- preparation process of the prior method. First, ferritin is isolated; more specifically, it is immobilized by immunoprecipitation with rabbit antihuman polyclonal antibody bound to agarose beads. The ferritin is then separated from other iron-containing proteins and free iron by a series of centrifugation and wash steps. Next, the ferritin is digested with nitric acid to extract its iron content. Finally, a micronebulizer is used to inject the sample of the product of the digestion into the ICPMS for analysis of its iron content. The sensitivity of the ICP-MS is high enough to enable it to characterize samples smaller than those required in the prior method (samples can be 0.15 to 0.60 mL).

Smith, Scott M.↗
DOE OSTI2011

Functionalization/passivation of porous graphitic carbon with di-tert-amylperoxide

Porous graphitic carbon (PGC) particles were functionalized/passivated in situ in packed beds at elevated temperature with neat di-tert-amylperoxide (DTAP) in a column oven. The performance of these particles for high performance liquid chromatography (HPLC) was assayed before and after this chemistry with the following analytes: benzene, toluene, ethyl benzene, n-propyl benzene, n-butyl benzene, p-xylene, phenol, 4-methylphenol, phenetole, 3,5-xylenol, and anisole. After the first functionalization/passivation, the retention factors, k, of these compounds decreased by about 5% and the number of theoretical plates (N) increased by ca. 15%. These values of k then remained roughly constant after a second functionalization/ passivation but a further increase in N was noticed. In addition, after each of the reactions, the peak asymmetries decreased by ca. 15%, for a total of ca. 30%. The columns were then subjected twice to methanol at 100 C for 5 h at 1 mL/min. After these stability tests, the values of k remained roughly constant, the number of plates increased, which is favorable, and the asymmetries rose and then declined, where they remained below the initial values for the unfunctionalized columns. Functionalized and unfunctionalized particles were characterized by scanning electron microscopy and BET measurements, which showed no difference between the functionalized and unfunctionalized materials, and X-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectrometry (ToF-SIMS), where ToF-SIMS suggested some chemical differences between the functionalized and unfunctionalized materials. In particular ToF-SIMS suggested that the expected five-carbon fragments from DTAP exist at higher concentrations on DTAP-functionalized PGC. First principle calculations on model graphitic surfaces suggest that the first addition of a DTAP radical to the surface proceeds in an approximately isothermal or slightly favorable fashion, but that subsequent DTAP additions are then increasingly thermodynamically favorable. Thus, this analysis suggests that the direct functionalization/passivation of PGC with DTAP is plausible. Chemometric analyses of the chromatographic and ToF-SIMS data are also presented.

10 SYNTHETIC FUELS↗
DOE OSTI2021

Defect–Concentration–Mediated T–Nb 2 O 5 Anodes for Durable and Fast–Charging Li–Ion Batteries

Metastable orthorhombic niobium pentoxide (T-Nb 2 O 5 ) is a promising anode to fulfill the requirements for high-rate Li-ion batteries (LIBs). Stoichiometric T-Nb 2 O 5 is plagued by low electric conductivity and particle pulverization after repeated charge/discharge processes. In this work, oxygen vacancies are implanted into T-Nb 2 O 5 particles via acid immersion of Nb 2 O 5 ·nH 2 O with the formation of Lewis acid sites. The multiple characterizations and simulations reveal the lengthening of Nb–O bonds, and the transformation from NbO 7 pentagonal bipyramids and NbO 6 tetragonal bipyramids in T-Nb 2 O 5–x . The enrichment of oxygen vacancies endows T-Nb 2 O 5–x with higher electric conductivity, better electrochemical kinetics, larger pseudocapacitive contribution. O-doped graphitic C 3 N 4 is creatively proposed as a trace oxygen pump to repair excessive oxygen vacancies, and it also serves as a sacrifice template for Nb 2 O 5–x growth to construct a porous and monolithic electrode network. Defect-modulated Nb 2 O 5–x displays extraordinary cycling stability (164 mAh g –1 at 5 C after 1100 cycles), high capacity retention (104 mAh g –1 ) at an ultrahigh rate (25 C), and large areal capacity (0.74 mAh cm –2 ) under high mass loading (4 mg cm –2 ). The practical prospect is proved by Nb 2 O 5–x /LiNi 0.8 Co 0.1 Mn 0.1 O 2 full cells with high average platform (2.12 V) and high specific capacity (229 mAh g –1 ). Finally, the oxygen-defect modulation strategy on oxide anodes provides an alternative solution to fast-charging and durable LIBs.

25 ENERGY STORAGE↗
DOE OSTI2019

Challenges and opportunities towards fast-charging battery materials

Extreme fast charging, with a goal of 15 minutes recharge time, is poised to accelerate mass market adoption of electric vehicles, curb greenhouse gas emissions and, in turn, provide nations with greater energy security. However, the realization of such a goal requires research and development across multiple levels, with battery technology being a key technical barrier. The present-day high-energy lithium-ion batteries with graphite anodes and transition metal oxide cathodes in liquid electrolytes are unable to achieve the fast-charging goal without negatively affecting electrochemical performance and safety. Here we discuss the challenges and future research directions towards fast charging at the level of battery materials from mass transport, charge transfer and thermal management perspectives. Additionally, we highlight advanced characterization techniques to fundamentally understand the failure mechanisms of batteries during fast charging, which in turn would inform more rational battery designs.

25 ENERGY STORAGE↗
NASA NTRS2001

Equivalent-Continuum Modeling of Nano-Structured Materials

A method has been developed for modeling structure-property relationships of nano-structured materials. This method serves as a link between computational chemistry and solid mechanics by substituting discrete molecular structures with an equivalent-continuum model. It has been shown that this substitution may be accomplished by equating the vibrational potential energy of a nano-structured material with the strain energy of representative truss and continuum models. As an important example with direct application to the development and characterization of single-walled carbon nanotubes, the model has been applied to determine the effective continuum geometry of a graphene sheet. A representative volume element of the equivalent-continuum model has been developed with an effective thickness. This effective thickness has been shown to be similar to, but slightly smaller than, the interatomic spacing of graphite.

Odegard, Gregory M.↗
NASA NTRS1992

Material characterization of composite laminates using low-frequency plate wave dispersion data

A recently developed ultrasonic techique which has been successful in monitoring the integrity of advanced structures is described. The technique is based on a two-transducer contact type arrangement that can be used to determine the dispersion curves of guided waves generated within the specimen. The phase velocity of antisymmetric plate waves is determined through spectral analysis of signals recorded from a lead break source on the surface of graphite epoxy laminates. The influence of all five stiffness constants on the dispersion curves of both symmetric and antisymmetric plate waves is theoretically investigated for propagation at 0, 45, and 90 deg to the fibers. All but c12 were found to have a strong influence on the dispersion curves in this frequency range. The fit with the theoretically predicted dispersion curves was excellent for propagation parallel and perpendicular to the fibers in the unidirectional specimen and good for the other cases considered.

Mal, Ajit K.↗
DOE OSTI2017

Economically Viable “Green” Carbon Anodes for Lithium-ion Batteries from Recycled Scrap Tires

The technical objective of this technical collaboration small business voucher (SBV) proposal was to develop methods at Oak Ridge National Laboratory (ORNL) to reduce the surface area and impurity contents present in the recovered carbon from scrap tires. Recycled tires have been used to make low-cost carbon anodes for lithium-ion batteries (LIB) with a cost-reduction of over 11-12%. Graphite is being used as the anode in LIBs. Oak Ridge National Laboratory (ORNL) has successfully recovered carbon composites from recycled tires with a yield of over 50% and demonstrated the electrochemical performance in a coin lithium ion cell configuration as an active anode material better than commercial graphite anode batteries [1]. ORNL has tailored the morphology of carbon powders from shredded recycled tires using a sulfonation process followed by pyrolysis to produce a highly value-added product and demonstrated its feasibility in LIBs. ORNL developed the methods to reduce impurities and surface area and provided carbon to Lawrence Berkley National Laboratory (LBNL) for detailed characterizations including lithium-ion battery testing. This SBV pilot project will also provide R&D infrastructure to FWD:Energy, Inc. (FWD) to establish a pre-pilot process to scale-up the synthesis of carbon composites from recycled tires and illustrate a high value commodity for anodes in large format LIBs.

25 ENERGY STORAGE↗
NASA NTRS1977

Fracture surface characteristics of off-axis composites

The fracture surface characteristics of off-axis high-modulus graphite-fiber/epoxy composite specimens were studied using a scanning electron microscope (SEM). The specimens were subjected to tensile loading at various angles (0-90 deg) to the fiber direction. SEM photomicrographs of the fractured surfaces revealed three different load angle regions with distinct fracture characteristics. Based on these revelations, criteria were established which can be used to characterize fracture surfaces with respect to a predominant 'single-stress' fracture mode.

Sinclair, J. H.↗