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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 415 records · Page 23

Toughening of Boron Carbide Composites by Hierarchical Microstructuring

Due to a unique combination of properties including high hardness, low density, chemical and thermal stability, semi-conductivity, and high neutron absorption, boron carbide (B4C) is a potential candidate for various applications involving extreme environment. However, B4C’s current application is limited because of its low fracture toughness. In this study, a hierarchical microstructure design with features including TiB2 grains and graphite platelets was used to toughen B4C by simultaneously utilizing multiple toughening mechanisms including crack deflection, bridging, and micro-crack toughening. Using field-assisted sintering technology (FAST), B4C composites with dense and hierarchical microstructure were fabricated. Previously, the fracture toughness of fabricated B4C composites was measured at micro-scale using micro-indentation to have up to 56% improvement. In this work, the B4C composites’ fracture toughness was characterized at macro-scale using four-point bending methods and compared with previous results obtained at micro-scale. Micromechanics modeling of fracture behaviors for B4C-TiB2 composites was also performed to evaluate the contributions from experimentally observed toughening mechanisms. From four-point bending tests, B4C composites reinforced with both TiB2 grains (~15 vol%) and graphite platelets (~8.7 vol%) exhibited the highest fracture toughness enhancement from 2.38 to 3.65 MPa∙m^(1/2). The measured values were lower than those obtained using micro-indentation but maintained the general trends. The discrepancy between the indentation and four-point bending test results originated from the complex deformation behaviors triggered by the high contact load during indentation tests. Through micromechanics modeling, introduced thermal residual stress due to thermal expansion mismatch between B4C and TiB2, and weak interphases at B4C-TiB2 boundaries were identified as the main causes for experimentally observed toughness enhancement. These results proved the effectiveness of hierarchical microstructure designs for B4C toughening and can provide reference for the future design of B4C composites with optimized microstructures for further fracture toughness enhancement.

composites↗

Mineralogical Characterization of Vigarano Matrix: HRTEM and EFTEM Observations

HRTEM and EFTEM have been used to study Vigarano matrix. Fine-grained rim olivines commonly contain inclusions of amorphous carbon and a Ca-Al-rich phase, whereas olivines in the clastic matrix contain rare inclusions of poorly graphitized carbon. Additional information is contained in the original extended abstract.

Abreu, N. M.↗

Moiré nematic phase in twisted double bilayer graphene

Graphene moiré superlattices display electronic flat bands. At integer fillings of these flat bands, energy gaps due to strong electron-electron interactions are generally observed. However, the presence of other correlation-driven phases in twisted graphitic systems at non-integer fillings is unclear. Here, we report the existence of threefold rotational symmetry breaking in twisted double bilayer graphene. Using spectroscopic imaging over large and uniform areas to characterize the direction and degree of C 3 symmetry breaking, we find it to be prominent only at energies corresponding to the flat bands and nearly absent in the remote bands. We demonstrate that the magnitude of the rotational symmetry breaking does not depend on the degree of the heterostrain or the displacement field, being instead a manifestation of an interaction-driven electronic nematic phase. We show that the nematic phase is a primary order that arises from the normal metal state over a wide range of doping away from charge. Furthermore, our modelling suggests that the nematic instability is not associated with the local scale of the graphene lattice, but is an emergent phenomenon at the scale of the moiré lattice.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Single-particle chemical analysis reveals organic-rich detonation soot products

The detonation of high explosives produces a wide variety of particulate matter (PM) with distinct properties, not all of which are traditionally studied for chemical composition, formation processes, and forensic applications. We report particle-resolved measurements of Composition B detonation soot using soot particle aerosol mass spectrometry (SP-AMS), identifying carbonaceous species and metals not previously characterized on a single-particle basis. Results are combined with scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) to enhance source-dependent signatures. Black carbon, including graphitic carbon and detonation nanodiamonds, contributed 50.5-71.4% of PM 2.5 mass, while 22.5-43.4% was non-refractory organic carbon, a previously overlooked component that exhibited a complex and varying composition. Detonations were performed with and without PMMA confinement and under steady and overdriven conditions. Distinct particles enriched with polycyclic aromatic hydrocarbons (PAHs) were observed in experiments utilizing confinement, with quantities dependent on manufacturing method. SEM-EDS validated SP-AMS findings of metals internally mixed with carbonaceous species and extended the particle size range to 100 µm. This work makes detecting non-refractory organics using single-particle techniques more feasible for detonation forensics and understanding high-energy soot formation. While this analysis uses offline sample collection, SP-AMS could be deployed for in-situ measurements of detonation PM 2.5 transported in the atmosphere.

36 MATERIALS SCIENCE↗

Graphite fiber textile preform/copper matrix composites

Graphite fiber reinforced/copper matrix composites have sufficiently high thermal conduction to make them candidate materials for critical heat transmitting and rejection components. The term textile composites arises because the preform is braided from fiber tows, conferring three-dimensional reinforcement and near net shape. The principal issues investigated in the past two years have centered on developing methods to characterize the preform and fabricated composite and on braidability. It is necessary to have an analytic structural description for both processing and final property modeling. The structure of the true 3-D braids used is complex and has required considerable effort to model. A structural mapping has been developed as a foundation for analytic models for thermal conduction and mechanical properties. The conductivity has contributions both from the copper and the reinforcement. The latter is accomplished by graphitization of the fibers, the higher the amount of graphitization the greater the conduction. This is accompanied by an increase in the fiber modulus, which is desirable from a stiffness point of view but decreases the braidability; the highest conductivity fibers are simply too brittle to be braided. Considerable effort has been expended on determining the optimal braidability--conductivity region. While a number of preforms have been fabricated, one other complication intervenes; graphite and copper are immiscible, resulting in a poor mechanical bond and difficulties in infiltration by molten copper. The approach taken is to utilize a proprietary fiber coating process developed by TRA, of Salt Lake City, Utah, which forms an itermediary bond. A number of preforms have been fabricated from a variety of fiber types and two sets of these have been infiltrated with OFHC copper, one with the TRA coating and one without. Mechanical tests have been performed using a small-scale specimen method and show the coated specimens to have superior mechanical properties. Final batches of preforms, including a finned, near net shape tube, are being fabricated and will be infiltrated before summer.

Gilatovs, G. J.↗

Electrochemical-driven green recovery of lithium, graphite and cathode from lithium-ion batteries using water

The expected exponential increase in consumption of lithium-ion batteries (LIBs) would pose a unique challenge to the availability of near-critical resources like lithium and graphite in the upcoming decade. In this work, we present a lithium recovery process that utilizes a degradation mechanism, i.e., lithium plating, as a tool to concentrate metallic lithium at the anode/separator interface for convenient extraction at room temperature – using only water. Electrochemical characterization of fast charged (1–6 C) LIBs yielded a maximum capacity fade of 50% over ten cycles. The lithium plating was confirmed via voltage plateau analysis, coulombic efficiency, and DC resistance measurements. A maximum lithium plating condition was observed to exist between 4C and 5C, thereby limiting the energy consumption in the extraction process. Post-mortem film thickness measurement showed an incrementing film deposition with a maximum of 35 µm thickness. SEM and XPS analysis confirmed increasing concentration of a dense dendritic metallic lithium deposition on the anode/separator interface with C-rate. A green recovery process was adopted to extract the concentrated metallic lithium using distilled water. The lithium from the plated film, solid/electrolyte interface (SEI), electrolyte, anode, and cathode, was extracted as salts. A 37% improvement in lithium recoverability was achieved with fast charging under ambient conditions. XPS analysis showed ~92% of lithium yield with no residual lithium in the graphite. In addition, the battery-grade graphite was recovered with 97% purity after heat treatment of the washed anode film, and concentrated transition metals oxides in the cathode to 93% purity for convenient extraction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

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↗

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.↗

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↗

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↗

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.↗

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.↗

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.↗

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.↗

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.↗

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.↗

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↗