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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 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Post Irradiation Examination Results of the NT-02 Graphite Fins NUMI Target

The NT-02 neutrino target in the NuMI beamline at Fermilab is a 95 cm long target made up of segmented graphite fins. It is the longest running NuMI target, which operated with a 120 GeV proton beam with maximum power of 340 kW, and saw an integrated total proton on target of 6.1 1020. Over the last half of its life, gradual degradation of neutrino yield was observed until the target was replaced. The probable causes for the target performance degradation are attributed to radiation damage, possibly including cracking caused by reduction in thermal shock resistance, as well as potential localized oxidation in the heated region of the target. Understanding the long-termstructural response of target materials exposed to proton irradiation is critical as future proton accelerator sources are becoming increasingly more powerful. As a result, an autopsy of the target was carried out to facilitate post-irradiation examination of selected graphite fins. Advanced microstructural imaging and surface elemental analysis techniques were used to characterize the condition of the fins in an effort to identify degradation mechanisms, and the relevant findings are presented in this paper.

43 PARTICLE ACCELERATORS↗
DOE OSTI2015

Multilayer graphane synthesized under high hydrogen pressure

A new hydrocarbon – hydrographite – with the composition close to CH is shown to form from graphite and gaseous hydrogen at pressures above 2 GPa and temperatures from 450 to 700 °C. Hydrographite is a black solid thermally stable under ambient conditions. When heated in vacuum, it decomposes into graphite and molecular hydrogen at temperatures from 500 to 650 °C. Powder X-ray diffraction characterizes hydrographite as a multilayer “graphane II” phase predicted by ab initio calculations [Wen X-D et al. PNAS 2011; 108:6833] and consisting of graphane sheets in the chair conformation stacked along the hexagonal c axis in the -ABAB- sequence. The crystal structure of the synthesized phase belongs to the P63mc space group. Moreover, the unit cell parameters are a = 2.53(1) Å and c = 9.54(1) Å and therefore exceed the corresponding parameters of graphite by 2.4(2)% and 42.0(3)%. Stretching vibrations of C–H groups on the surface of the hydrographite particles are examined by infrared spectroscopy.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Measurement of anode surface temperature in carbon nanomaterial production by arc discharge method

Highlights: • We measured the temperature of anode surface by two-color pyrometry combined with a high speed camera successfully. • Growth temperature of pyrolytic graphite, MWNTs, and nano-graphite particles were in ranges of 2400–2600 K, 2600–2700 K, and 2700–3500 K, respectively. • High temperature contributes to form thermodynamically unstable material. - Abstract: Nano-graphite particles, multi-wall carbon nanotube (MWNT), and pyrolytic graphite were prepared at different positions of the anode surface in an arc discharge. Graphite electrodes were employed for the arc discharge under helium environment at atmospheric pressure. Nano-sized carbon products were characterized by scanning electron microscopy and transmission electron microscopy. During the arc discharge, two-color pyrometry combined with a high-speed camera was conducted to measure the temperature distribution of the anode surface. The growth temperature of pyrolytic graphite, MWNT, and nano-graphite particles were in the ranges of 2400–2600 K, 2600–2700 K, and 2700–3500 K, respectively. The local temperature of anode surface is a critical parameter to determine the products with different morphologies. The formation mechanism of these carbon nanomaterials is suggested based on the local temperature of anode surface and their thermodynamic stability.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Synthesis and CO{sub 2} adsorption study of modified MOF-5 with multi-wall carbon nanotubes and expandable graphite

MOF-5 was synthesized by solvothermal method and its reactivation under anhydrous conditions. This research is conducted to investigate the effect of MOF-5 and MOF-5 modified with multi-wall carbon nanotubes (MWCNTs) and expandable graphite (EG) on the performance of CO{sub 2} adsorption. The synthesized MOFs were characterized using Field emission scanning electron microscopy (FESEM) for surface morphology, Thermogravimetric analysis (TGA) for thermal stability, X-ray diffraction (XRD) for crystals plane, Brunauer-Emmet-Teller (BET) for surface area and CO{sub 2} adsorption. The result had showed that the modified MOF-5 enhanced the CO{sub 2} adsorption compared to the pure MOF-5. The increment in the CO{sub 2} uptake capacities of MOF materials was attributed to the decrease in the pore size and enhancement of micropore volume of MOF-5 by multi-walled carbon nanotube and EG incorporation. The BET surface area of the synthesized MOF-5@MWCNTs is more than MOF-5. The CO{sub 2} sorption capacities of MOF-5 and MOF-5@MWCNTs were observed to increase from 0.00008 to 0.00048 mol g-1 at 298 K and 1 bar. The modified MOF-5@MWCNTs resulted in the highest CO{sub 2} adsorption followed by the modified MOF-5@ EG and lastly, MOF-5.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Neutron Reference Benchmark Field Specifications: ACRR Polyethylene-Lead-Graphite (PLG) Bucket Environment (ACRR-PLG-CC-32-CL)

This report was put together to support the International Atomic Energy Agency (IAEA) REAL- 2016 activity to validate the dosimetry community’s ability to use a consistent set of activation data and to derive consistent spectral characterizations. The report captures details of integral measurements taken in the Annular Core Research Reactor (ACRR) central cavity with the Polyethylene-Lead-Graphite (PLG) bucket, reference neutron benchmark field. The field is described and an “a priori” calculated neutron spectrum is reported, based on MCNP6 calculations, and a subject matter expert (SME) based covariance matrix is given for this “a priori” spectrum. The results of 37 integral dosimetry measurements in the neutron field are reported.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2023

Enhanced Electrochemical Performance of Disordered Rocksalt Cathodes Enabled by a Graphite Conductive Additive

Cobalt-free cation-disordered rocksalt (DRX) cathodes are a promising class of materials for next-generation Li-ion batteries. Although they have high theoretical specific capacities (>300 mA h/g) and moderate operating voltages (~3.5 V vs Li/Li + ), DRX cathodes typically require a high carbon content (up to 30 wt %) to fully utilize the active material which has a detrimental impact on cell-level energy density. To assess pathways to reduce the electrode’s carbon content, the present study investigates how the carbon’s microstructure and loading (10–20 wt %) influence the performance of DRX cathodes with the nominal composition Li 1.2 Mn 0.5 Ti 0.3 O 1.9 F 0.1 . While electrodes prepared with conventional disordered carbon additives (C65 and ketjenblack) exhibit rapid capacity fade due to an unstable cathode/electrolyte interface, DRX cathodes containing 10 wt % graphite show superior cycling performance (e.g., reversible capacities ~260 mA h/g with 85% capacity retention after 50 cycles) and rate capability (~135 mA h/g at 1000 mA/g). Furthermore, a suite of characterization tools was employed to evaluate the performance differences among these composite electrodes. Overall, these results indicate that the superior performance of the graphite-based cathodes is largely attributed to the: (i) formation of a uniform graphitic coating on DRX particles which protects the surface from parasitic reactions at high states of charge and (ii) homogeneous dispersion of the active material and carbon throughout the composite cathode which provides a robust electronically conductive network that can withstand repeated charge–discharge cycles. Overall, this study provides key scientific insights on how the carbon microstructure and electrode processing influence the performance of DRX cathodes. Based on these results, exploration of alternative routes to apply graphitic coatings is recommended to further optimize the material performance.

25 ENERGY STORAGE↗
DOE OSTI2017

Portable Vibro-acoustic Testing System for In Situ Microstructure Characterization and Metrology

Portable Vibro-acoustic Testing System for In situ Microstructure Characterization and Metrology James A. Smith, Corrie I. Nichol Idaho National Laboratory, Idaho Falls ID Mostafa Fatemi, Mayo Clinic, Rochester MN There is a need in research reactors like the INL to inspect irradiated materials and structures. The goal of this work is to develop a portable scanning infrastructure for a material characterization technique called vibro-acoustography (VA) that has been developed by INL [1] for nuclear applications to characterize fuel, cladding materials, and structures. The proposed VA technology is based on ultrasound and acoustic waves; however, it provides information beyond what is available from the traditional ultrasound techniques and can expand the knowledge on nuclear material characterization and microstructure evolution. VA is a three-dimensional (3D) imaging modality based on ultrasound-stimulated acoustic emission. VA uses the force caused by the beating of two frequencies to generate an acoustic emission signal. Due to absorption or reflection, the energy density in the object at an acoustic focal point changes to produce a “radiation force.” This force locally vibrates the object, which results in an acoustic field that depends on the characteristics of the object at that point. This acoustic field is detected for every point in the object; the resulting data is used to make an image of the object’s mechanical properties. This technology is fundamentally different from traditional ultrasound imaging. More specifically, VA is: (a) based on the “radiation force,” a nonlinear phenomenon in sound propagation, and (b) sensitive to both high and low frequency dynamic responses of the object. The combination of these two response types provides information about characteristics of the object beyond what is possible by traditional ultrasound imaging. High spatial resolution is achieved, since the radiation force is localized to the focal point of the ultrasound beam. Low-frequency information, which is a representative of structural characteristics, is gained through the radiation force mechanism at a low (beat) frequency. This paper will report on the development of a portable scanning that can be set up to characterize materials and component in open water reactors and canals in situ. We will show some initial laboratory results of images generated by vibro-acoustics of surrogate fuel plates and graphite structures and discus the design of the portable system. 1. Smith, J. A., and Kunerth, D. C., “Vibro-acoustic Sensors for Materials Characterization and Related Methods and Systems,” Patent Application 13226280, 09/06/2011.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Scalable Upcycling of Spent Lithium-Ion Battery Anodic Graphite to Electronic-Grade Graphene

Recycling processes for lithium-ion batteries (LIBs) are imperative to support the sustainable growth of global energy storage systems. This study introduces a scalable method for the upcycling of spent graphite anodes from LIBs to produce electronic-grade graphene nanoplatelets. In addition to comprehensive materials characterization, the electronic quality of the upcycled graphene is demonstrated by formulating it into a screen printing ink that achieves high-resolution patterning and thin-film electrical conductivity exceeding 104 S m−1. This screen printing ink is also used to print planar micro-supercapacitors with exceptional areal capacitance (1.78 mF cm−2), areal energy density (0.247 µWh cm−2), and cycling stability (> 10 000 cycles). Life cycle assessment (LCA) and techno-economic analysis (TEA) highlight the environmental benefits and cost reductions attainable through upcycling of graphite from LIBs. By capturing economic value from spent LIBs, this work fosters a sustainable battery supply chain and provides an abundant and geographically distributed raw material for electronic-grade graphene.

energy storage↗
DOE OSTI2014

Thermal plasma synthesis of Fe{sub 1−x}Ni{sub x} alloy nanoparticles

Fe-Ni alloy nanoparticles are of great interest because of diverse practical applications in the fields such as magnetic fluids, high density recording media, catalysis and medicine. We report the synthesis of Fe-Ni nanoparticles via thermal plasma route. Thermal plasma assisted synthesis is a high temperature process and gives high yields of production. Here, we have used direct arc thermal plasma plume of 6kw as a source of energy at operating pressure 500 Torr. The mixture of Fe-Ni powder in required proportion (Fe{sub 1−x}Ni{sub x}; x=0.30, 0.32, 0.34, 0.36, 0.38 and 0.40) was made to evaporate simultaneously from the graphite anode in thermal plasma reactor to form Fe-Ni bimetallic nanoparticles. The as synthesized particles were characterized by X-Ray Diffraction (XRD), Thermo-Gravimetric Analysis/Differential Scanning Calorimtry (TGA/DSC)

36 MATERIALS SCIENCE↗
DOE OSTI2024

Solvent-Mediated, Reversible Ternary Graphite Intercalation Compounds for Extreme-Condition Li-Ion Batteries

Traditional Li-ion intercalation chemistry into graphite anode exclusively utilizes the co-intercalation-free or co-intercalation mechanism. The latter mechanism is based on ternary graphite intercalation compounds (t-GICs), where glyme solvents were explored and proved to deliver unsatisfied cyclability in LIBs. Herein, we report a novel intercalation mechanism, that is, in-situ synthesis of t-THF-GICs in the tetrahydrofuran (THF) electrolyte via a spontaneous, controllable reaction between binary-GICs and free THF molecules during initial graphite lithiation. The spontaneous transformation from b-GIC to t-GIC, which is different from conventional co-intercalation chemistry, is characterized and quantified via operando synchrotron X-ray and electrochemical analyses. The resulting t-GIC chemistry obviates the necessity for complete Li-ion desolvation, facilitating rapid kinetics and synchronous charge/discharge of graphite particles even under high current densities. Consequently, the graphite anode demonstrates unprecedented fast charging (1 min), dendrite-free low-temperature performance, and ultralong lifetimes exceeding 10,000 cycles. Full cells coupled with layered cathode, display remarkable cycling stability upon a 15-min charging and excellent rate capability even at -40 °C. Furthermore, our chemical strategies are shown to extend beyond Li-ion batteries to encompass Na-ion and K-ion batteries, underscoring their broad applicability. Our work contributes to the advancement of graphite intercalation chemistry and presents a low-cost, adaptable approach to achieving fast-charging and low-temperature batteries.

25 ENERGY STORAGE↗
DOE OSTI2014

Nano-scale orientation mapping of graphite in cast irons

A diametrical section of a graphite spheroid from a ductile iron sample was prepared using the focused ion beam-lift out technique. Characterization of this section was carried out through automated crystal orientation mapping in a transmission electron microscope. This new technique automatically collects electron diffraction patterns and matches them with precalculated templates. The results of this investigation are crystal orientation and phase maps of the specimen, which bring new light to the understanding of growth mechanisms of this peculiar graphite morphology. This article shows that mapping the orientation of carbon-based materials such as graphite, which is difficult to achieve with conventional techniques, can be performed automatically and at high spatial resolution using automated crystal orientation mapping in a transmission electron microscope. - Highlights: • ACOM/TEM can be used to study the crystal orientation of carbon-based materials. • A spheroid is formed by conical sectors radiating from a central nuclei. • Misorientations exist within the conical sectors, defining various orientation domains.

36 MATERIALS SCIENCE↗
NASA NTRS1986

Mechanical properties characterization of composite sandwich materials intended for space antenna applications

The composite materials proposed for use in the Advanced Communications Technology Satellite (ACTS) Program contains a new, high modulus graphite fiber as the reinforcement. A study was conducted to measure certain mechanical properties of the new fiber-reinforced material as well as of a composite-faced aluminum honeycomb sandwich structure. Properties were measured at -157, 22, and 121 C. Complete characterization of this material was not intended. Longitudinal tensile, picture-frame shear, short-beam shear, and flexural tests were performed on specimens of the composite face-sheet materials. Unidirectional, cross-plied, and quasi-isotropic fiber composite ply layup designs were fabricated and tested. These designs had been studied by using NASA's Integrated Composite Analyzer (ICAN) computer program. Flexural tests were conducted on (+/- 60/0 deg) sub s composite-faced sandwich structure material. Resistance strain gages were used to measure strains in the tensile, picture-frame, and sandwich flexural tests. The sandwich flexural strength was limited by the core strength at -157 and 22 C. The adhesive bond strength was the limiting factor at 121 C. Adhesive mechanical properties are reflected in sandwich structure flexural properties when the span-to-depth ratio is great enough to allow a significant shear effect on the load-deflection behavior of the sandwich beam. Most measured properties agreed satisfactorily with the properties predicted by ICAN.

Bowles, Kenneth J.↗
NASA NTRS1989

Mechanical properties characterization of composite sandwich materials intended for space antenna applications

The composite materials proposed for use in the Advanced Communications Technology Satellite (ACTS) program contains a new, high modulus graphite fiber as the reinforcement. A study was conducted to measure certain mechanical properties of the new fiber-reinforced material as well as of a composite-faced aluminum honeycomb sandwich structure. Properties were measured at -157, 22, and 121 C. Complete characterization of this material was not intended. Longitudinal tensile, picture-frame shear, short-beam shear, and flexural tests were performed on specimens of the composite face-sheet materials. Unidirectional, cross-plied, and quasi-isotropic fiber composite ply layup designs were fabricated and tested. These designs had been studied by using NASA's Integrated Composite Analyzer (ICAN) computer program. Flexural tests were conducted on (+/- 60/0 deg) sub s composite-faced sandwich structure material. Resistance strain gages were used to measure strains in the tensile, picture-frame, and sandwich flexural tests. The sandwich flexural strength was limited by the core strength at 157 and 22 c. The adhesive bond strength was the limiting factor at 121 C. Adhesive mechanical properties are reflected in sandwich structure flexural properties when the span-to-depth ratio is great enough to allow a significant shear effect on the load-deflection behavior of the sandwich beam. Most measured properties agreed satisfactorily with the properties predicted by ICAN.

Bowles, Kenneth J.↗
DOE OSTI2018

Selecting the Best Graphite for Long-Life, High-Energy Li-Ion Batteries

Here, most lithium-ion batteries still rely on intercalation-type graphite materials for anodes, so it is important to consider their role in full cells for applications in electric vehicles. Here, we systematically evaluate the chemical and physical properties of six commercially-available natural and synthetic graphites to establish which factors have the greatest impact on the cycling stability of full cells with nickel-rich LiNi0.8Mn0.1Co0.1O2 (NMC811) cathodes. Electrochemical data and post-mortem characterization explain the origin of capacity fade. The NMC811 cathode shows large irreversible capacity loss and impedance growth, accounting for much of full cell degradation. However, six graphite anodes demonstrate significant differences with respect to structural change, surface area, impedance growth, and SEI chemistry, which impact overall capacity retention. We found long cycle life correlated most strongly with stable graphite crystallite size. In addition, graphites with lower surface area generally had higher coulombic efficiencies during formation cycles, which led to more stable long-term cycling. The best graphite screened here enables a capacity retention around 90% in full pouch cells over extensive long-term cycling compared to only 82% for cells with the lowest performing graphite. The results show that optimal graphite selection improves cycling stability of high energy lithium-ion cells.

25 ENERGY STORAGE↗
DOE OSTI2023

Disorder and hydrogenation in graphene nanopowder revealed by complementary X-ray and neutron scattering

Functionalization of graphene's two-dimensional sheets can be used to modify the physical properties of graphene, such as changing its conductivity or inducing ferromagnetism, which is of broad interest for a myriad of applications. However, functionalized graphene can possess significant structural disorder that is often overlooked and is difficult to characterize quantitatively. Here we investigate hydrogenated graphene nanopowder (H-Gr) produced by Birch reduction of graphene oxide. By combining complementary x-ray and neutron diffraction, we show how to quantitatively characterize the H-Gr nanostructure, including the hydrogen content. Further, we show that the majority of the H-Gr consists of highly disordered molecular-scale carbon while a small portion of the sample contains few-layered graphene having an expanded interlayer spacing. Modeling the coherent diffuse scattering for both x-ray and neutron diffraction, and comparing it with the incoherent neutron scattering, the hydrogen to carbon ratio was measured and it was determined that most of the hydrogen resides within the disordered carbon rather than in the graphene. Evidence is presented for hydrogen clustering as well as for hydrogen bonded perpendicular to the plane of molecular-carbon bonds. Our quantitative approach to characterizing carbon nanopowders has broad relevance to understanding disorder and bonding of hydrogen in graphitic carbons and other nanomaterials.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Extending carbon chemistry at high-pressure by synthesis of CaC 2 and Ca 3 C 7 with deprotonated polyacene- and para-poly(indenoindene)-like nanoribbons

Metal carbides are known to contain small carbon units similar to those found in the molecules of methane, acetylene, and allene. However, for numerous binary systems ab initio calculations predict the formation of unusual metal carbides with exotic polycarbon units, [C 6 ] rings, and graphitic carbon sheets at high pressure (HP). Here we report the synthesis and structural characterization of a HP-CaC 2 polymorph and a Ca 3 C7 compound featuring deprotonated polyacene-like and para-poly(indenoindene)-like nanoribbons, respectively. We also demonstrate that carbides with infinite chains of fused [C6] rings can exist even at conditions of deep planetary interiors (~140 GPa and ~3300 K). Hydrolysis of high-pressure carbides may provide a possible abiotic route to polycyclic aromatic hydrocarbons in Universe.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Bonding, elastic and vibrational properties in low and high pressure synthesized diamond-like BCx phases

Recent studies demonstrate that low pressure chemical vapor deposition at 950 K leads to the synthesis of diamond-like boron carbides with high concentrations of boron (0.66 < x < 4) in which the sp 2 fraction depends on the boron concentration [1]. This indicates that the graphitic BC3 (g-BC3) phases obtained by chemical vapor deposition materials are mixtures of diamond-like and graphitic BCx phases. This finding allows us to revise the interpretation of the x-ray diffraction (XRD) patterns of the g-BC3 phases discussed previously [2, 3]. To support the new interpretation, we conducted a laser heating experiment of the g-BC3 phase. We found that after laser heating at 1100 K and 25 GPa in a diamond anvil cell (DAC) almost all graphitic layers of the g-BC3 transform into a cubic structure. The XRD pattern of the cubic BC3 phase (c-BC3) can be indexed with a cubic unit cell a = 3.619 (0.165) Å. Measurements of the equation of state of the g-BC3 phase demonstrated that boron atoms were incorporated into the graphitic B-C network. The linear compressibility along the c axis can be characterized by the value of the linear modulus Bc = 29.2 ± 1.8 GPa. Linear fitting of the experimental data for the a/a o parameter as a function of pressure gives us the value of the linear elastic modulus along the a axes: Ba = 800 ± 75 GPa.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
NASA NTRS1980

Spatial distribution of volatile compounds in graphite composites

The distribution of water and other volatile compounds such as acetone and phenol was measured as a function of depth in four graphite resin matrix composites. Precision abrasion mass spectrometry was used to qualitatively and quantitatively characterize the indigenous volatile compounds in the as received condition and after drying in an environmentally controlled oven. The total amount of water in the composites varied from 0.12 wt% to 1.1 wt% and the times required to dry the samples ranged from less than 96 h to much greater than 555 h.

Grayson, M. A.↗