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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 703 records · Page 39
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Superconducting magnesium diboride films for levitation of laser targets

Inertial confinement fusion targets would benefit from being levitated inside hohlraums to avoid capsule support-related implosion perturbations. Levitation inside a magnetic trap requires coating the capsule with a thin film that is superconducting at 20 K. Such non-epitaxial film growth on non-planar substrates is challenging. Here, we study Mg vapor annealing and solid-phase reactive inter-diffusion methods to form superconducting magnesium diboride (MgB 2 ) films on different planar and spherical carbon substrates, evaluating glassy carbon, polycrystalline diamond made by chemical vapor deposition, and carbon deposited by magnetron sputtering of graphite targets. Thin films of B and Mg are produced by magnetron sputtering onto stationary planar or rolling spherical substrates and annealed at either 600 or 850 °C in Mg vapor. The films are characterized by a combination of high-energy ion scattering, electron microscopy, and magnetometry. Results show that the critical superconducting temperature of resultant films depends on film microstructure and oxygen impurity content. The formation of MgB 2 films is also strongly substrate dependent, even in this case of non-epitaxial growth. Important factors to consider are oxygen outgassing of the substrate during thermal processing, substrate surface roughness, and the matching of thermal expansion coefficients of different layers in the multilayer structure.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

The many phases of CaC{sub 2}

Polymorphic CaC{sub 2} was prepared by reacting mixtures of CaH{sub 2} and graphite with molar ratios between 1:1.8 and 1:2.2 at temperatures between 700 and 1400 °C under dynamic vacuum. These conditions provided a well controlled, homogeneous, chemical environment and afforded products with high purity. The products, which were characterized by powder X-ray diffraction, solid state NMR and Raman spectroscopy, represented mixtures of the three known polymorphs, tetragonal CaC{sub 2}-I and monoclinic CaC{sub 2}-II and -III. Their proportion is dependent on the nominal C/CaH{sub 2} ratio of the reaction mixture and temperature. Reactions with excess carbon produced a mixture virtually free from CaC{sub 2}-I, whereas high temperatures (above 1100 °C) and C-deficiency favored the formation of CaC{sub 2}-I. From first principles calculations it is shown that CaC{sub 2}-I is dynamically unstable within the harmonic approximation. This indicates that existing CaC{sub 2}-I is structurally/dynamically disordered and may possibly even occur as slightly carbon-deficient phase CaC{sub 2-δ}. It is proposed that monoclinic II is the ground state of CaC{sub 2} and polymorph III is stable at temperatures above 200 °C. Tetragonal I represents a metastable, heterogeneous, phase of CaC{sub 2}. It is argued that a complete understanding of the occurrence of three room temperature modifications of CaC{sub 2} will require a detailed characterization of compositional and structural heterogeneities within the high temperature form CaC{sub 2}-IV, which is stable above 450 °C. The effect of high pressure on the stability of the monoclinic forms of CaC{sub 2} was studied in a diamond anvil cell using Raman spectroscopy. CaC{sub 2}-II and -III transform into tetragonal CaC{sub 2}-I at about 4 and 1GPa, respectively. - Graphical abstract: The famous tetragonal form of CaC{sub 2}, CaC{sub 2}-I, is dynamically unstable. Why does it exist? Display Omitted - Highlights: • Critical review of complex polymorphism of the commodity chemical CaC{sub 2}. • Tetragonal CaC{sub 2}-I is identified as dynamical instable and its existence attributed to disorder. • With pressure monoclinic CaC{sub 2}-II and –III transform into tetragonal CaC{sub 2}-I. • The high temperature form CaC{sub 2}-IV is assigned a key role for understanding the polymorphism of CaC{sub 2}.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Carbonaceous Material Properties and Their Interactions with Slag During Electric Arc Furnace Steelmaking

The state of the interface between slag and carbon determines the slag foaming behavior and thus the effectiveness of carbon in electric arc furnace (EAF) steelmaking. This paper explores the interaction between synthetic slag and carbonaceous materials derived from various sources, including bio-char produced by two different technologies, graphite, coke, and char from tire pyrolysis. Different interfacial phenomena were found between slag and the carbonaceous materials examined. The interactions between bio-char and slag are found to be poor in comparison with other carbonaceous materials. Carbonaceous materials were characterized in terms of their chemical composition and the results obtained suggested that interfacial phenomena were not dominated by ash in the carbonaceous material. The effects of carbon crystalline structure on interaction with slag were evaluated by Raman spectroscopy and X-ray diffraction. Surface properties of the samples were evaluated using scanning electron microscopy, and surface morphology was identified as the principal factor affecting the interaction of slag on carbonaceous particles. The smooth surface of bio-char results in reduced slag foaming. This finding forms the basis for future research on the production of bio-char to be used as a slag foaming agent in EAF steelmaking.

36 MATERIALS SCIENCE↗
DOE OSTI2010

Effect of Air Oxidation on Pore Structure Development and Mechanical Properties of Nuclear Graphite

This document reports on continuation of R&D activities at ORNL directed at investigating the effect of air oxidation of nuclear graphite on development and structure of porosity in the oxidized layer, and on the effect on mechanical properties of oxidized graphite. The material investigated was nuclear-grade graphite (purified PCEA graphite, from GrafTech International). Based on conclusions of previous work (ORNL/TM-2009/192), the method of analysis of the porosity in the oxidized layer based on optical microscopy coupled with automated image analysis was further improved and standardized. In addition, characterization of oxidized specimens by optical microscopy was complemented with measurements of mechanical properties (compressive strength) on a statistically significant number of specimens. A series of cylindrical shape specimens were machined and oxidized in air at two temperatures (600 and 700 o C) and at three levels of burn-off at each temperature (5-6 %; 10-12 % and 15-17%). The procedure used for specimen preparation and oxidation, and the oxidation equipment, were those recommended in ASTM D-7542-09. However, in order to comply with the aspect ratio requirements for specimens employed in compressive strength measurements (ASTM C-695-91) all specimens were machined with a length to diameter ratio of 2 (i.e. 25.4 mm height vs. 12.7 mm diameter) instead of 25.4 mm length and 25.4 mm diameter recommended by ASTM D-7542-09. After oxidation, mechanical properties (compressive strength) were measured on at least three samples obtained at equal oxidation conditions, while another specimen from the same lot was sectioned, mounted in resin and surface polished for optical microscopy analysis. In the latter procedure, mosaic pictures were collected of a rectangular stripe across the diameter of each specimen. These images were analyzed in order to derive the penetration depth and the pore structure in the oxidized layer as a function of oxidation temperature and weight loss level. Automated image analysis was performed using the commercial software Image Pro Plus. The results led to the conclusion that the depth of the oxidation layer is more dependent on the oxidation temperature than on the level of weight-loss. The penetration depth of the oxidized layer is about 6 mm at 600 o C and about 1.5 mm at 700 o C. Consequently, the 12.5 mm diameter specimens oxidized at 600 o C were completely penetrated by oxidation, while those oxidized at 700 o C had the oxidation layer restricted in a narrower band near the exposed surface. This difference was reflected by mechanical properties. A closer analysis of high magnification images in the oxidized layer revealed that oxidation attacks preferentially the binder phase in graphite, where development of fine new pores was observed. The density of new pores was higher near large pores pre-existing in graphite structure. Acute oxidation at low temperatures (e.g. 600 o C) causes more damage on mechanical strength than high temperature oxidation (700 o C). Although the latter is much faster, the oxidized layer is limited to a narrow zone next to the external surface, so that the core is not visibly affected. In contrast, oxidation at lower temperature, although slower, is more damaging because it penetrates deeply beyond the exposed surface.

36 MATERIALS SCIENCE↗
NASA NTRS2000

Experimental and Numerical Characterization of a Steady-State Cylindrical Blackbody Cavity at 1100 Degrees Celsius

A blackbody calibration furnace at the NASA Dryden Flight Research Center is used to calibrate heat flux gages. These gages are for measuring the aerodynamic heat flux on hypersonic flight vehicle surfaces. The blackbody is a graphite tube with a midplane partition which divides the tube into two compartments (dual cavities). Electrical resistance heating is used to heat the graphite tube. This heating and the boundary conditions imposed on the graphite tube result in temperature gradients along the walls of the blackbody cavity. This paper describes measurements made during steady-state operation and development of finite-difference thermal models of the blockbody furnace at 1100 C. Two configurations were studied, one with the blackbody outer surface insulated and the other without insulation. The dominant modes of heat transfer were identified for each configuration and the effect of variations in material properties and electric current that was passed through the blackbody were quantified.

Horn, Thomas J.↗
DOE OSTI2021

Mesoporous Textured Fe-N-C Electrocatalysts as Highly Efficient Cathodes for Proton Exchange Membrane Fuel Cells

A new platinum group metal (PGM)-free proton exchange membrane fuel cell (PEMFC) cathode catalyst materials, synthesized using the VariPore™ method by Pajarito Powder, LLC, are characterized for their structure and activity. The physico-chemical analysis of the iron-nitrogen-carbon (Fe-N-C) electrocatalysts show mesoporous carbon material effectively doped with iron and nitrogen. The materials have an average pore size of 7-8 nm and high specific surface area. The Fe-N-C catalysts exhibit good oxygen reduction reaction (ORR) activity in 0.5 M H2SO4 electrolyte with high half-wave potential and sustainable electrochemical stability over 10,000 repeated potential cycles with insignificant losses in their activities. As cathode catalysts in a PEMFC, the Fe-N-C materials deliver remarkably good fuel cell performance at low overpotential approaching that of the commercial Pt catalyst. The high ORR electrocatalytic activity of these Fe-N-C catalysts is credited to the synergy between nitrogen-moieties, specifically pyrrolic-N, pyridinic-N, and graphitic-N, and iron in addition to the high mesoporosity that facilitate an effective reaction path in boosting the electrocatalytic activity and stability.

DIRECT ENERGY CONVERSION↗
DOE OSTI2010

A novel nanostructured composite formed by interaction of copper octa(3-aminopropyl)octasilsesquioxane with azide ligands: Preparation, characterization and a voltammetric application

This study presents the preparation, characterization and application of copper octa(3-aminopropyl)octasilsesquioxane following its subsequent reaction with azide ions (ASCA). The precursor (AC) and the novel compound (ASCA) were characterized by Fourier transform infrared spectra (FTIR), nuclear magnetic resonance (NMR), electron paramagnetic resonance (EPR), scanning electronic microscopy (SEM), X-ray diffraction (XRD), Thermogravimetric analyses and voltammetric technique. The cyclic voltammogram of the modified graphite paste electrode with ASCA (GPE-ASCA), showed one redox couple with formal potential (E{sub 1/2}{sup ox}) = 0.30 V and an irreversible process at 1.1 V (vs. Ag/AgCl; NaCl 1.0 M; v=20mVs{sup -1}). The material is very sensitive to nitrite concentrations. The modified graphite paste electrode (GPE-ASCA) gives a linear range from 1.0 x 10{sup -4} to 4.0 x 10{sup -3} mol L{sup -1} for the determination of nitrite, with a detection limit of 2.1 x 10{sup -4} mol L{sup -1} and the amperometric sensitivity of 8.04 mA/mol L{sup -1}.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Capacitive deionization using carbon derived from an array of zeolitic-imidazolate frameworks

Capacitive deionization (CDI) represents one of the most thermodynamically efficient technologies for brackish water desalination. Its performance is highly reliant on the surface properties of carbon-based electrodes. Zeolitic-imidazolate framework (ZIF)-derived carbon materials have emerged among the most promising candidates owing to their high structural and compositional tuneability. However, the impacts of the precursory ZIF structure on the properties of the final carbon, and therefore, CDI capacity and efficiency remain to be further explored. In this work, four Zn-based ZIFs with different side-chain substitutions on the imidazolates were synthesized on a gram scale with high yields to produce N-doped carbons by pyrolysis. Next, the resulting carbons along with four commercial carbon blacks were characterized physically and electrochemically to explore the structure-performance relationship. We demonstrated that the imidazole side-chain substitution alters the ZIF's decomposition during pyrolysis, influencing the elemental compositions, surface properties, wettability and graphitization levels. The diverse carbon properties result in variable double layer capacitance and charge-transfer resistance, ultimately impacting the CDI performance. Among these carbons, Zn (4abIm)2-C afforded the greatest salt adsorption capacity of 14.19 mg NaCl $·g_C^{–1}$, while Zn (mIm) 2 -C showed the highest overall salt adsorption capacity and rate; both exceeded the performance of the commercial carbon blacks.

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

Direct Visualization of Solid Electrolyte Interphase Formation in Lithium-Ion Batteries with In Situ Electrochemical Transmission Electron Microscopy

Complex, electrochemically driven transport processes form the basis of electrochemical energy storage devices. The direct imaging of electrochemical processes at high spatial resolution and within their native liquid electrolyte would significantly enhance our understanding of device functionality, but has remained elusive. In this work we use a recently developed liquid cell for in situ electrochemical transmission electron microscopy to obtain insight into the electrolyte decomposition mechanisms and kinetics in lithium-ion (Li-ion) batteries by characterizing the dynamics of solid electrolyte interphase (SEI) formation and evolution. Here we are able to visualize the detailed structure of the SEI that forms locally at the electrode/electrolyte interface during lithium intercalation into natural graphite from an organic Li-ion battery electrolyte. We quantify the SEI growth kinetics and observe the dynamic self-healing nature of the SEI with changes in cell potential.

25 ENERGY STORAGE↗
DOE OSTI2014

Solid Radiochemistry Nuclear Diagnostic Results from Exploding Pusher Shot (N130503-002) at the National Ignition Facility

The Solid Radiochemistry (SRC) nuclear diagnostic platform has been developed for the assessment of various performance parameters, such as areal fuel density and ablator-fuel mixing, associated with the capsule implosion of DT-fuel, hohlraum based shots at the National Ignition Facility (NIF). This diagnostic is based on the collection and characterization of debris from the capsule and surrounding materials (primarily gold from the hohlraum). SRC utilizes two diagnostic instrument manipulators (DIMs), 90-78 and 0-0, to field debris collectors (maximum of four metallic and/or graphite foils per DIM) inside the NIF chamber during shots. The debris collectors are removed after a shot and transferred to the Nuclear Counting Facility (NCF) for the measurement of gold activation (Au-196m and Au-196) and capture (Au-198) products via gamma spectroscopy. The results from SRC which show a strong dependency on an independently measured neutron down scatter ratio (DSR) are utilized as part of a 1-D capsule model to determine the areal densities (ρR(DT) and ρR(CH)) during burn. This report summarizes the SRC results from the Indirect Drive Exploding Pusher shot (N130503-002) designed to produce low ρR at burn time (~40 mg/cm 2 ) leading to a significant decrease in DSR (0.23±0.07 %). As a result, this shot is considered a calibration shot for SRC nuclear diagnostic.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
NASA NTRS1978

A biaxial method for inplane shear testing

A biaxial method for performing inplane shear tests of materials using a shear frame is described. Aluminum plate and sandwich specimens were used to characterize the uniformity of shear strain imparted by the biaxial method of loading as opposed to the uniaxial method. The inplane stiffening effect of aluminum honeycomb core was determined. Test results for (+ or - 45) graphite-epoxy laminate are presented. Some theoretical considerations of subjecting an anisotropic material to a uniform shear deformation are discussed.

Bush, H. G.↗
NASA NTRS1977

Heat exchanger-ingot casting/slicing process, phase 1: Silicon sheet growth development for the large area silicon sheet task of the low cost silicon solar array project

A controlled growth, heat-flow and cool-down process is described that yielded silicon with a high degree of single crystallinity. Even when the seed melted out, very large grains formed. Solar cell samples made from cast material yielded conversion efficiency of over 9%. Representative characterizations of grown silicon demonstrated a dislocation density of less than 100/sq cm and a minority carrier diffusion length of 31 micron. The source of silicon carbide in silicon ingots was identified to be from graphite retainers in contact with silica crucibles. Higher growth rates were achieved with the use of a graphite plug at the bottom of the silica crucible.

Schmid, F.↗
NASA NTRS1981

Tribological properties and surface chemistry of silicon carbide at temperatures to 1500 C

Silicon carbide surfaces were heated to 1500 C in a vacuum and analyzed at room temperature with X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). The basic unit of the surfaces was considered as a plane of a tetrahedron of either SiC4 and CSi4 composition. AES spectra were obtained from 250-1500 C, with an analysis depth of 1 nm revealed the presence of little Si and mostly graphite. XPS analysis depth was 2 nm or less, and Si was found in the second 1 nm. Sliding friction tests with single-crystal silicon carbide in contact with iron in a vacuum were characterized by a stock-slip value. The coefficient of friction increased with increasing temperature up to 400 C, then decreased with increasing temperature from 400-600 C. Reheating surfaces to 800 C after preheating them to that temperature produced no changes in AES readings. It is concluded that the maximum density of silicon and silicon-carbide is at 800 C, and the higher the sliding temperature, the more metal that is transferred.

Miyoshi, K.↗
NASA NTRS1986

Tetraglycidyl epoxy resins and graphite fiber composites cured with flexibilized aromatic diamines

Studies were performed to synthesize new ether modified, flexibilized aromatic diamine hardeners for curing epoxy resins. The effect of moisture absorption on the glass transition temperatures of a tetraglycidyl epoxy, MY 720, cured with flexibilized hardeners and a conventional aromatic diamine was studied. Unidirectional composites, using epoxy-sized Celion 6000 graphite fiber as the reinforcement, were fabricated. The room temperature and 300 F mechanical properties of the composites, before and after moisture exposure, were determined. The Mode I interlaminar fracture toughness of the composites was characterized using a double cantilever beam technique to calculate the critical strain energy release rate.

Delvigs, P.↗
NASA NTRS1991

Advanced materials for space nuclear power systems

The overall philosophy of the research was to develop and characterize new high temperature power conversion and radiator materials and to provide spacecraft designers with material selection options and design information. Research on three candidate materials (carbide strengthened niobium alloy PWC-11 for fuel cladding, graphite fiber reinforced copper matrix composites for heat rejection fins, and tungsten fiber reinforced niobium matrix composites for fuel containment and structural supports considered for space power system applications is discussed. Each of these types of materials offers unique advantages for space power applications.

Titran, Robert H.↗
NASA NTRS1991

Advanced materials for space nuclear power systems

The overall philosophy of the research was to develop and characterize new high temperature power conversion and radiator materials and to provide spacecraft designers with material selection options and design information. Research on three candidate materials (carbide strengthened niobium alloy PWC-11 for fuel cladding, graphite fiber reinforced copper matrix composites for heat rejection fins, and tungsten fiber reinforced niobium matrix composites for fuel containment and structural supports) considered for space power system applications is discussed. Each of these types of materials offers unique advantages for space power applications.

Titran, Robert H.↗
NASA NTRS1991

Characterization of the dimensional stability of advanced metallic materials using an optical test bench structure

The dimensional stability of low-density high specific-strength metal-matrix composites (including 30 vol pct SiC(p)/SXA 24-T6 Al, 25 vol pct SiC(p)/6061-T6 Al, 40 vol pct graphite P100 fiber/6061 Al, 50 vol pct graphite P100 fiber/6061 Al, and 40 vol pct P100 graphite fiber/AZ91D Mg composites) and an Al-Li-Mg metal alloy was evaluated using a specially designed five-strut optical test bench structure. The structure had 30 thermocouple locations, one retroreflector, one linear interferometer multilayer insulation, and various strip heaters. It was placed in a 10 exp -7 torr capability vacuum chamber with a laser head positioned at a window port, and a laser interferometer system for collecting dimensional change data. It was found that composite materials have greater 40-C temporal dimensional stability than the AL-Li-Mg alloy. Aluminum-based composites demonstrated better 40-C temporal stability than Mg-based composites.

Hsieh, Cheng↗