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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 397 records · Page 22
All sourcesNASA NTRSDOE OSTI
NASA NTRS1996

An acoustic emission and acousto-ultrasonic analysis of impact damaged composite pressure vessels

The use of acoustic emission to characterize impact damage in composite structures is being performed on composite bottles wrapped with graphite epoxy and kevlar bottles. Further development of the acoustic emission methodology will include neural net analysis and/or other multivariate techniques to enhance the capability of the technique to identify dominant failure mechanisms during fracture. The acousto-ultrasonics technique will also continue to be investigated to determine its ability to predict regions prone to failure prior to the burst tests. Characterization of the stress wave factor before, and after impact damage will be useful for inspection purposes in manufacturing processes. The combination of the two methods will also allow for simple nondestructive tests capable of predicting the performance of a composite structure prior to its being placed in service and during service.

Workman, Gary L.↗
DOE OSTI2016

Microstructural Characterization of In-reactor Corrosion Tested Hastelloy N{sup R} and 316 Stainless Steel

The success of the Molten Salt Reactor Experiment (MSRE) at the Oak Ridge National Laboratory (ORNL) in the period 1950's-70's has rekindled the interested in molten salt-cooled reactors. The most recent form of this type of reactor, the Fluoride salt-cooled High-temperature nuclear Reactors (FHRs) is emerging as a leading reactor concept for the next generation nuclear reactors because it offers, among other benefits, a high degree of passive safety, high thermal efficiency, and low spent fuel. Since 2011, two three-year Integrated Research Projects (IRPs) were awarded by the U. S. Department of Energy (DoE) to the Massachusetts Institute of Technology (MIT) in partnership with the University of California, Berkeley and the University of Wisconsin-Madison to develop a 'path forward' for the development of the FHR. One primary challenge in these projects is to evaluate the corrosion and compatibility of structural alloys in the potential primary coolant of molten Li{sub 2}BeF{sub 4} (FLiBe) salt at 700 deg. C in a neutron irradiation environment. In support of structural materials development for the FHR, the static in-reactor corrosion tests of two promising alloys, nickel-based Hastelloy N{sup R} and 316 stainless steel, in {sup 7}Li-enriched molten FLiBe have been conducted in both metal-lined and graphite crucibles in the MIT nuclear research reactor in 2013. This work focuses on the microstructural characterization of the in-reactor corrosion tested alloys for understanding of their performance in high-temperature molten FLiBe salt. Our preliminary results indicate significant thermal effects, graphite effects, and irradiation effects on the alloys' performance in high-temperature molten FLiBe salt, particularly for the in-reactor corrosion tests. The neutron irradiation induces tritium generation in molten salt which could combine with fluorine ions to form corrosive HF to dramatically attack alloys. Additionally, the neutron irradiation introduces structural defects into alloys which probably alter alloys' corrosion resistivity to high temperature molten FLiBe salt. The effect of graphite on the alloys' corrosion in a nuclear reactor is also possibly different from the out-of-reactor corrosion. All these issues will be better understood by characterizing the microstructure of in-reactor corrosion tested alloy samples in our near future plans. The experimental data in this study provides valuable input for evaluating structural materials performance in the FHR. (authors)

36 MATERIALS SCIENCE↗
DOE OSTI2017

Understanding the reaction of nuclear graphite with molecular oxygen: Kinetics, transport, and structural evolution

A thorough understanding of oxidation is important when considering the health and integrity of graphite components in graphite reactors. For the next generation of graphite reactors, HTGRs specifically, an unlikely air ingress has been deemed significant enough to have made its way into the licensing applications of many international licensing bodies. While a substantial body of literature exists on nuclear graphite oxidation in the presence of molecular oxygen and significant efforts have been made to characterize oxidation kinetics of various grades, the value of existing information is somewhat limited. Often, multiple competing processes, including reaction kinetics, mass transfer, and microstructural evolution, are lumped together into a single rate expression that limits the ability to translate this information to different conditions. This article reviews the reaction of graphite with molecular oxygen in terms of the reaction kinetics, gas transport, and microstructural evolution of graphite. It also presents the foundations of a model for the graphite-molecular oxygen reaction system that is kinetically independent of graphite grade, and is capable of describing both the bulk and local oxidation rates under a wide range of conditions applicable to air-ingress.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

Understanding the Reaction of Nuclear Graphite with Molecular Oxygen

A thorough understanding of oxidation is important when considering the health and integrity of graphite components in graphite reactors. For the next generation of graphite reactors, HTGRs specifically, an unlikely air ingress has been deemed significant enough to have made its way into the licensing applications of many international licensing bodies. While a substantial body of literature exists on nuclear graphite oxidation in the presence of molecular oxygen and significant efforts have been made to characterize oxidation kinetics of various grades, the value of existing information is somewhat limited. Often, multiple competing processes, including reaction kinetics, mass transfer, and microstructural evolution, are lumped together into a single rate expression that limits the ability to translate this information to different conditions. This article reviews the reaction of graphite with molecular oxygen in terms of the reaction kinetics, gas transport, and microstructural evolution of graphite. It also presents the foundations of a model for the graphite-molecular oxygen reaction system that is kinetically independent of graphite grade, and is capable of describing both the bulk and local oxidation rates under a wide range of conditions applicable to air-ingress.

J. Kane, Joshua↗
DOE OSTI2023

Determining the oxidation behavior of matrix graphite

This work presents the oxidation behavior of matrix graphite in air. Matrix graphite, graphite powder/flakes bonded by a small amount of non-graphitic carbon, surrounds coated fuel particles in order to form cylindrical fuel compacts (in prismatic core designs) or spheres (in pebble-bed reactor designs). This work focuses on oxidation tests conducted on two matrix graphite materials, one provided by Kairos Power and the other A3 matrix graphite. Some of the tests followed American Society for Testing and Materials (ASTM) oxidation testing standards using a vertical furnace system and others were performed in a thermogravimetric analyzer (TGA). It was determined that, at temperatures of 450 °C–700 °C, the oxidation rate of the Kairos matrix graphite follows the Arrhenius equation. In comparison with A3 matrix graphite, the Kairos matrix graphite shows better oxidation resistance at high temperatures (≥550 °C), but also a higher oxidation rate at low temperatures. Both the A3 matrix graphite and the Kairos matrix graphite materials may experience preferential oxidation of the partially graphitized binder. An oxygen penetration gradient was also observed when using the three characterization methods (i.e., optical microscope, x-ray tomography [XCT], and density profile by the lathe) enlisted in this research. In conclusion, the oxygen penetration depth increases with decreasing isothermal oxidation temperature, while the center of the oxidized samples (10% weight loss) remains almost untouched even at 500 °C.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2016

TH-CD-BRA-10: Towards Reference Dosimetry of MR-Linacs Using a Clinical Probe-Format Calorimeter

Purpose: To evaluate the influence of a 1.5 T magnetic field (B-field) on the response of a small-scale graphite calorimeter probe (GPC) developed for use as a novel clinical reference dosimeter. Characterization of the GPC was also assessed in a hybrid MRI-linac (MRL) clinical prototype by performing absolute dosimetry in multiple detector orientations. Methods: B-field influence was characterized using a variable-strength electromagnet system located 280 cm from the source of a clinical linac. The GPC was used to perform a total of 160 absolute dose measurements (6 MV, 920 MU/min) in a water phantom placed between the poles of the electromagnet. The magnitude of the B-field between the poles was varied in the range of 0 – 1.5 T. The relative response of the GPC was determined and compared to that of a thimble type ionization chamber (Exradin A1SL, Standard Imaging). Next, 65 dose measurements were performed using the GPC in a clinical MRL field (7 MV, 620 MU/min) to quantify the rotational dependence of the detector in the presence of a 1.5 T B-field. The GPC was rotated in steps of 90° inside a graphite phantom (SSD 140 cm, depth 2.5 cm) for two detector orientations (parallel and perpendicular to the B field). Results: Relative to the zero B-field condition, the A1SL chamber exhibited an average overresponse of +1.2 % ± 0.03 % at a B-field of 1.5 T, while the GPC under-responded on average by −0.5 % ± 0.9 %. For the MRL measurements, no significant differences were observed between the parallel and perpendicular orientations. In both cases, a rotational dependence of approximately ±1 % was measured. Conclusion: This work suggests that the B-field has minimal influence on the response of the GPC, making it a potentially attractive solution for clinical MRL reference dosimetry. This work has been supported in part by the CREATE Medical Physics Research Training Network NSERC grant RGPIN 432290, as well as NSERC grants RGPIN 298191 & 435608. JR is a scholar from The Terry Fox Foundation Strategic Training Initiative for Excellence in Radiation Research for the 21st Century (EIRR21).

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
NASA NTRS2015

Characterization of Organic Materials in the Xenolithic Clasts in Sharps (H3.4) Meteorite Using Micro-Raman Spectroscopy

Graphitization of carbon is an irreversible process which alters the structure of graphitic materials in response to the increase in metamorphic grade (temperature and/or pressure). Carbonaceous materials offer a reliable geothermometer as their Raman spectra change systematically with increasing metamorphic grade. In this study, we identified carbonaceous materials in the xenolithic clasts in Sharps and interpreted their metamorphic history by revealing the structural organization (order) of the polyaromatic organic phases using micro-Raman spectroscopy.

Chan, Q. H. S.↗
NASA NTRS1990

Aeolian removal of dust from radiator surfaces on Mars

Simulated radiator surfaces made of arc-textured Cu and Nb-1 percent-Zr and ion beam textured graphite and C-C composite were fabricated and their integrated spectral emittance characterized from 300 to 3000 K. A thin layer of aluminum oxide, basalt, or iron (III) oxide dust was then deposited on them, and they were subjected to low pressure winds in the Martian Surface Wind Tunnel. It was found that dust deposited on simulated radiator surfaces may or may not seriously lower their integrated spectral emittance, depending upon the characteristics of the dust. With Al2O3 there is no appreciable degradation of emittance on a dusted sample, with basaltic dust there is a 10 to 20 percent degradation, and with Fe2O3 a 20 to 40 percent degradation. It was also found that very high winds on dusted highly textured surfaces can result in their abrasion. Degradation in emittance due to abrasion was found to vary with radiator material. Arc-textured Cu and Nb-1 percent Zr was found to be more susceptible to emittance degradation than graphite or C-C composite. The most abrasion occurred at low angles, peaking at the 22.5 deg test samples.

Gaier, James R.↗
DOE OSTI2021

Key Features of Polyimide‐Derived Carbon Molecular Sieves

Abstract Carbon molecular sieve (CMS) membranes have impressive separation properties; however, both chemical and morphology structures need to be understood better. Here we characterize CMS with the simplest polyimide (PI) PMDA/pPDA (PMDA=pyromellitic dianhydride, pPDA= p ‐phenylenediamine), using FTIR, solid‐state 15 N‐NMR and 13 C‐NMR, XPS, XRD, and Raman spectra to study chemical structure. We also compare gas separation properties for this CMS to a CMS derived from a more conventional PI precursor. The detailed characterization shows the presence of aromatic pyridinic, pyrrolic rings as well as graphitic, pyridonic components and a few other groups in both CMS types derived from the very different precursors. The CMS morphologies, while related to precursor and pyrolysis temperature details, show similarities consistent with a physical picture comprising distributed molecular sieving plate‐like structures. These results assist in understanding diverse CMS membrane separation performance.

Qiu, Wulin↗
DOE OSTI2021

Key Features of Polyimide-Derived Carbon Molecular Sieves

Carbon molecular sieve (CMS) membranes have impressive separation properties; however, both chemical and morphology structures need to be understood better. Here we characterize CMS with the simplest polyimide (PI) PMDA/pPDA (PMDA=pyromellitic dianhydride, pPDA=p-phenylenediamine), using FTIR, solid-state 15 N-NMR and 13 C-NMR, XPS, XRD, and Raman spectra to study chemical structure. Here we also compare gas separation properties for this CMS to a CMS derived from a more conventional PI precursor. The detailed characterization shows the presence of aromatic pyridinic, pyrrolic rings as well as graphitic, pyridonic components and a few other groups in both CMS types derived from the very different precursors. The CMS morphologies, while related to precursor and pyrolysis temperature details, show similarities consistent with a physical picture comprising distributed molecular sieving plate-like structures. These results assist in understanding diverse CMS membrane separation performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Determination of the “NiOOH” charge and discharge mechanisms at ideal activity

Here, optimization of electrodeposition conditions produced Ni(OH) 2 deposits chargeable up to 1.84 ± 0.02 e – per Ni on and the resulting nickel oxide/hydroxide active material could subsequently deliver 1.58 ± 0.02 e – per Ni ion (462 mA h/g) over a potential range <0.2 V. The ability of the “NiOOH” active material to deliver an approximately ideal charge and discharge facilitated a coulometric and thermodynamic analysis through which the charge/discharge mechanisms were determined from known enthalpies of formation. The (dis)charge states were confirmed with in situ Raman spectroscopy. The mechanisms were additionally evaluated with respect to pH and potential dependence, charge quantities, hysteresis, and fluoride ion partial inhibition of the charge mechanism. The results indicate that the “NiOOH” (dis)charges as a solid-state system with mechanisms consistent with known nickel and oxygen redox reactions. A defect chemistry mechanism known for the LiNiO 2 system also occurs for “NiOOH” to cause both high activity and hysteresis. Similar to other cation insertion nickel oxides, the activity of the “NiOOH” mechanism is predominantly due to oxygen redox activity and does not involve the Ni4 + oxidation state. The “NiOOH” was produced from cathodic electrodeposition of Ni(OH) 2 from nickel nitrate solutions onto highly oriented pyrolytic graphite at ideal electrodeposition current efficiencies and the deposition mechanism was also characterized.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2017

Insights on the extraordinary tolerance to alcohols of Fe-N-C cathode catalysts in highly performing direct alcohol fuel cells

Direct alcohol fuel cells (DAFCs) represent the best alternative to batteries for portable and auxiliary power units application due to the high energy density of short chain alcohols. Currently, the utilization of the best platinum group metal (PGM) cathode catalysts is limited, not only by a high cost and scarce resources, but also by the inefficient oxygen reduction reaction (ORR) when permeated alcohols adsorb on the catalytic active sites. In this work, a highly active Fe-N-C catalyst derived from the pyrolysis of nicarbazin (a nitrogen charge transfer organic salt) and an iron precursor has been investigated to get insights on the extraordinary tolerance to the presence of alcohols (methanol and ethanol) of such a PGM-free catalyst. Density functional theory (DFT) calculations demonstrate for the first time that Fe-N 4 and Fe-N 2 C 2 active sites preferentially adsorb oxygen with much higher energy than methanol, ethanol and products of partial ethanol oxidation (0.73–1.16 eV stronger adsorption), while nitrogen-carbon related sites (pyridinic and graphitic nitrogen) are much less selective towards ORR. Half-cell electrochemical characterization showed that the Fe-N-C catalyst overcomes Pt ORR activity in acidic medium with methanol or ethanol concentrations as low as 0.01 M. The feasibility of DAFCs operation based on high methanol (up to 17 M) and ethanol (up to 5 M) concentration thanks to the utilization of Fe-N-C cathode catalyst is demonstrated. Lastly, a new strategy is proposed for DAFCs where using Pt only at the anode and Fe-N-C at the cathode allows extending the device energy density compared to PGM-based catalysts at both electrodes.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2023

Ab initio structural dynamics of pure and nitrogen-containing amorphous carbon

Abstract Amorphous carbon (a-C) has attracted considerable interest due to its desirable properties, which are strongly dependent on its structure, density and impurities. Using ab initio molecular dynamics simulations we show that the sp 2 /sp 3 content and underlying structural order of a-C produced via liquid quenching evolve at high temperatures and pressures on sub-nanosecond timescales. Graphite-like densities ( $$\lesssim$$ ≲ 2.7 g/cc) favor the formation of layered arrangements characterized by sp 2 disordered bonding resembling recently synthesized monolayer amorphous carbon (MAC), while at diamond-like densities ( $$\gtrsim$$ ≳ 3.3 g/cc) the resulting structures are dominated by disordered tetrahedral sp 3 hybridization typical of diamond-like amorphous carbon (DLC). At intermediate densities the system is a highly compressible mixture of coexisting sp 2 and sp 3 regions that continue to segregate over 10’s of picoseconds. The addition of nitrogen (20.3%) (a-CN) generates major system features similar with those of a-C, but has the unexpected effect of reinforcing the thermodynamically disfavored carbon structural motifs at low and high densities, while inhibiting phase separation in the intermediate region. At the same time, no nitrogen elimination from the carbon framework is observed above $$\simeq$$ ≃ 2.8 g/cc, suggesting that nitrogen impurities are likely to remain embedded in the carbon structures during fast temperature quenches at high pressures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Examining Performance Loss Mechanisms in Lithium-Ion Batteries with the High-Voltage Mn-Rich Spinel Positive Electrodes

The high-voltage spinel, with the nominal composition of LiNi 0.5-x Mn 1.5+x O 4 (LNMO), could be a sustainable alternative to the layered-oxide positive electrodes used in lithium-ion batteries. However, commercial acceptance has been limited as LNMO cells display rapid performance loss during cycling. To examine reasons for this loss we prepared cells with LNMO-based positive and either graphite or lithium titanate (LTO) based negative electrodes. Our initial cells displayed high impedance and rapid impedance rise during cycling. Adding single walled carbon nanotubes in the positive lowered initial cell impedance but impedance increased during cycling because of coating delamination from the Al foil. Using a primed Al current collector solved the delamination problem: cells with this current collector showed only a small impedance rise. Regarding capacity, cells with the LTO negative showed higher initial capacities and smaller fade. Our data indicate that cell capacity retention is determined by reduction reactions at the negative electrode that lower capacity and oxidation reactions at the positive electrode that increase capacity: both types of reactions deplete the cell electrolyte during extended cycling. All things considered, species generated at high voltages, either in the electrolyte or at the LNMO electrode, drive cell capacity fade.

25 ENERGY STORAGE↗
DOE OSTI2018

Microwave-Driven Plasma-Mediated Methane Cracking: Product Carbon Characterization

Methane is the primary industrial H 2 source, with the vast majority produced by steam reforming of methane—a highly CO 2- and water-intensive process. Alternatives to steam reforming, such as microwave-driven plasma-mediated methane decomposition, offer benefits of no water consumption and zero CO 2 process emissions while also producing solid carbon formed by pyrolytic reactions and aided by a plasma reactive environment. The economic viability of pyrolytic methane decomposition as a hydrogen source will depend upon the commercial applications of the solid carbon product—which, in turn, will depend upon its physical and chemical characteristics. This study focuses on material characterization of the solid carbon (secondary) product. Characterization by high-resolution transmission electron microscopy reveals forms ranging from graphitic to amorphous. Thermogravimetric analyses reveal three forms by their differing oxidative reactivity, while X-ray diffraction analyses support the different crystalline forms as suggested by Thermogravimetric analysis. Plasma perturbation of the radical pool, elevating radical temperatures and boosting concentrations, is proposed as altering the reaction paths towards solid carbon formation, resulting in the different sp 2 forms.

42 ENGINEERING↗
NASA NTRS1980

Characterization of aging effects of LARC-160

Specimens of freshly prepared polyimide precursor resin LARC-160 and resin aged at room temperature up to 45 days were characterized by high-pressure liquid chromatography and several different thermal analyses. Graphite reinforced composites were then fabricated from fresh and aged resin and tested to determine if changes observed by these techniques were significant. It was found that resin aging resulted in greater flow during processing and poorer composite isothermal stability. However, aging did not affect the room-temperature flexural or short-beam-shear strengths of the composites.

Young, P. R.↗
DOE OSTI2014

High Yield Synthesis of Mesoscopic Conductive and Dispersible Carbon Nanostructures via Ultrasonication of Commercial Precursors

The need to produce large quantities of graphenic materials displaying excellent conductivity, thermal resistance, and tunable properties for industrial applications has spurred interest in new techniques for exfoliating graphite. In this paper, sonication-assisted exfoliation of graphitic precursors in the presence of chloroform is shown to produce chemically and structurally unique exfoliated graphitic materials in high yields. These exfoliated graphites, referred to as mesographite and mesographene, respectively, exhibit unique properties which depend on the number of layers and exfoliation conditions. Structural characterization of mesographene reveals the presence of nanoscale two-dimensional graphene layers, and threedimensional carbon nanostructures sandwiched between layers, similar to those found in ball-milled and intercalated graphites. The conductivities of mesographite and mesographene are 2700 and 2000 S/m, respectively, indicating high conductivity despite flake damage. Optical absorption measurements of mesographite sonicated in various solvents showed significant changes in dispersion characteristics, and also indicated significant changes to mesoscopic colloidal behavior. A mechanism for functionalization and formation of capped carbon nanostructures is proposed by integrating the chemical and structural characterization in relation to the various carbon structures observed by electron microscopy. Composites based on common polymers were prepared by solution processing, and changes in thermal properties indicate improved dispersion of mesographite in polar polymers.

Srivastava, Vikram K↗
DOE OSTI2025

Graphite crystals in catalytically-graphitized glass-like carbon

Catalytic graphitization of glass-like carbon leads to enhanced growth of micro-sized graphitic crystals with unusual shapes of wires, filaments, tubes, rods, whiskers, and spirals. Similar particles with axial symmetry are also found in pure glass-like carbon heat-treated at high temperatures. Nonetheless, the presence of a graphitization catalyst, Si in this case, in the heat-treatment process supports the transformation of porous, disordered carbon structure towards the graphitic atomic order and the formation of manifold peculiar polyhedral wires and particles of geometry distinct from the plate-like shape typical for conventional graphite. In contrast to conventional carbon nanotubes and fibers, the graphene layers are stacked perpendicular to the tube axis, while the size of the most common tube fibers can reach up to 10 μm in diameter and 100 μm in length. X-ray diffraction, Raman spectroscopy, scanning and transmission electron microscopy, small-angle X-ray scattering combined with complementary techniques have been used to characterize the structure of the glass-like carbon derived from furfuryl alcohol catalytically-graphitized using Si particles at 3000 °C. Finally, since control of graphite shape is vital to achieving the level of performance required in contemporary applications, the obtained results demonstrate that the catalytic graphitization method may be employed to produce filamentous graphite crystals.

36 MATERIALS SCIENCE↗