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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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The development of titanium matrix composites for elevated temperature applications was investigated. General solutions for treating diffusion in multiphase multicomponent systems were studied. Graphite polyimide composites were characterized with respect to mechanical property degradation by moisture.
New analytical techniques and a processability laminate have been used in the development of a material specification for 350 F curing epoxy-graphite materials. The development of the specification required the evaluation of prepregs which had variations in their processing behavior that were detected only in production. Chemical techniques were used to analyze the prepregs and establish limits on the concentrations of the various chemical constituents. A batch acceptance test laminate was designed to determine suitability of prepregs for production useage. The new specification requires that the processability laminate be ultrasonically and micrographically inspected for voids and porosity. Incorporation of these and other requirements will help to insure material consistency and processability.
Molten salts, such as lithium fluoride, are attractive candidates for thermal energy storage in solar dynamic space power systems because of their high latent heat of fusion. However, these same salts have poor thermal conductivities which inhibit the transfer of heat into the solid phase and out of the liquid phase. One concept for improving the thermal conductivity of the thermal energy storage system is to add a conductive filler material to the molten salt. High thermal conductivity pitch-based graphite fibers are being considered for this application. Although there is some information available on the thermal conductivity of lithium fluoride solid, there is very little information on lithium fluoride liquid, and no information on molten salt graphite fiber composites. This paper describes a hot filament technique for determining the thermal conductivity of molten salts. The hot filament technique was used to find the thermal conductivity of molten lithium fluoride at 930 C, and the thermal conductivity values ranged from 1.2 to 1.6 W/mK. These values are comparable to the slightly larger value of 5.0 W/mK for lithium fluoride solid. In addition, two molten salt graphite fiber composites were characterized with the hot filament technique and these results are also presented.
This research effort focused on the use of eddy current techniques for characterizing flaws in graphite-based filament-wound cylindrical structures. A major emphasis was on incorporating artificial intelligence techniques into the signal analysis portion of the inspection process. Developing an eddy current scanning system using a commercial robot for inspecting graphite structures (and others) has been a goal in the overall concept and is essential for the final implementation for expert system interpretation. Manual scans, as performed in the preliminary work here, do not provide sufficiently reproducible eddy current signatures to be easily built into a real time expert system. The expert systems approach to eddy current signal analysis requires that a suitable knowledge base exist in which correct decisions as to the nature of the flaw can be performed. In eddy current or any other expert systems used to analyze signals in real time in a production environment, it is important to simplify computational procedures as much as possible. For that reason, we have chosen to use the measured resistance and reactance values for the preliminary aspects of this work. A simple computation, such as phase angle of the signal, is certainly within the real time processing capability of the computer system. In the work described here, there is a balance between physical measurements and finite element calculations of those measurements. The goal is to evolve into the most cost effective procedures for maintaining the correctness of the knowledge base.
The use of eddy current techniques for characterizing flaws in graphite-based filament-wound cylindrical structures is described. A major emphasis was also placed upon incorporating artificial intelligence techniques into the signal analysis portion of the inspection process. Developing an eddy current scanning system using a commercial robot for inspecting graphite structures (and others) was a goal in the overall concept and is essential for the final implementation for the expert systems interpretation. Manual scans, as performed in the preliminary work here, do not provide sufficiently reproducible eddy current signatures to be easily built into a real time expert system. The expert systems approach to eddy current signal analysis requires that a suitable knowledge base exist in which correct decisions as to the nature of a flaw can be performed. A robotic workcell using eddy current transducers for the inspection of carbon filament materials with improved sensitivity was developed. Improved coupling efficiencies achieved with the E-probes and horseshoe probes are exceptional for graphite fibers. The eddy current supervisory system and expert system was partially developed on a MacIvory system. Continued utilization of finite element models for predetermining eddy current signals was shown to be useful in this work, both for understanding how electromagnetic fields interact with graphite fibers, and also for use in determining how to develop the knowledge base. Sufficient data was taken to indicate that the E-probe and the horseshoe probe can be useful eddy current transducers for inspecting graphite fiber components. The lacking component at this time is a large enough probe to have sensitivity in both the far and near field of a thick graphite epoxy component.
This report summarizes the nondestructive microstructure characterization undertaken at Oak Ridge National Laboratory (ORNL) to understand the effects of high-temperature neutron irradiation on the structure of nuclear graphite. Nuclear graphite specimens were irradiated in the ORNL High Flux Isotope Reactor (HFIR) in the High Temperature Vehicle (HTV) with target irradiation temperatures of 900ºC, 1200ºC, and 1500ºC [1, 2]. The experiment was irradiated in the HFIR flux trap for two irradiation cycles, providing the specimens in the highest-fluence positions a total exposure of 4.5×10 21 n/cm 2 [E>0.1 MeV], equivalent to radiation damage of ~3.3 dpa (displacements per atom) according to the conversion factor in Burchell [3].
This paper summarizes the results of an investigation conducted to characterize tensile and shear response of P100/6061 graphite-aluminum composite in the temperature range -101 to 260 C. The off-axis tension test and Iosipescu shear test methods were employed to meet this objective. The experimental results indicate that both the fiber-dominated and matrix-dominated elastic properties exhibit relatively small changes in the considered temperature range. The effect of temperature on yielding and strength, however, is significant under longitudinal and shear loading. Residual stresses play a significant role in controlling the variation of the yield stress with temperature. The observed low transverse strength of the composite is explained by interfacial defects between adjacent precursor wires induced during fabrication.
This study investigates the graphitization process of polyacrylonitrile (PAN) carbon fibers by subjecting commercial fibers to thermal heat treatment at temperatures ranging from 1400 to 2100 °C in 100 °C increments, using either argon or nitrogen gas atmospheres. Changes in crystallinity, surface morphology, and lattice parameters were analyzed for two commercial carbon fibers using X-ray diffraction, scanning electron microscopy, and Raman spectroscopy. Results indicated minimal changes in surface morphology with increasing heat-treatment temperature; however, crystallinity significantly increased. Crystallinity changes were more strongly dependent on temperature rather than gas atmosphere or fiber type. At intermediate heat-treatment temperatures (1600–1800 °C), fibers treated in argon showed a slight preference for graphitization. The highest level of graphitization was measured at 2100 °C. Crystallite size increased as the intensity ratio of the D1 to G Raman peaks increased, reaching a peak around ~1800 °C, after which the ratio started to decrease. This behavior aligns with Ferrari's three-stage model of carbon crystallization and is consistent with both the Marie-Mering degree of graphitization and Brubaker's Integrated Absolute Differential models, all of which describe the transformation from an amorphous to a more graphitic structure. At the higher heat-treatment temperatures, the changes between atmospheres and fiber types were measured to converge to similar levels of graphitization. In conclusion, this study evaluates the progressive change in commercial grade carbon fibers when heat-treated.
NLR will help ACE Green Recycling evaluate and develop its processes for environmentally friendly and low-cost recycling of graphite, lithium-iron phosphate (LFP), and other cathode materials from spent lithium-ion batteries.
An experimental study has been carried out to prepare and characterize epoxy/amine-based composites filled with different percentages of partially exfoliated graphite (i.e. pEG) particles having an exfoliation degree of 56% in order to analyze the effect of the filler amounts on the electrical properties of the resulting nanocomposites. Moreover, in order to fully investigate the direct relationship between the physical properties of the employed filler and the results of the electrical characterization, a structural and morphological characterization of the pEG samples is carried out by means of various type of analysis such as X-ray diffraction patterns, micro-Raman and Scanning Electron Microscopy (SEM) images. The DC electrical characterization reveals a percolation thresholds (EPT) that falls in the range [2–3] wt% and an electrical conductivity of about 0.66 S/m at the highest filler loading (6.5 wt%). From the analysis of the percolative curve it is possible to derive the percolation law parameters and in particular the critical exponent t, whose value (i.e. 1.2) reflects an effective 2D organization of the percolating structure consistent with the type of filler used (2-dimensional). Finally, an extensive analysis concerning the electrical properties in the frequency domain has been carried out in order to evaluate the effectiveness of pEG-loaded composites in terms of electromagnetic interference compatibility (EMC) and their applicability as radar absorbers materials (RAMs).
This study characterizes the effects of electron radiation and temperature on a graphite-epoxy composite material. Compressive properties of the T300/934 material system were obtained at -250 F (-157 C), room temperature, and 250 F (121 C). Tensile specimens of the Fiberite 934 epoxy resin were fabricated and tested at room temperature and 250 F (121 C). Testing was conducted in the baseline (nonirradiated) and irradiated conditions. The radiation exposure was designed to simulate 30 year, worst-case exposure in geosynchronous Earth orbit. Mechanical properties tended to degrade at elevated temperature and improve at cryogenic temperature. Irradiation generally degraded properties at all temperatures.
An understanding of the underlying mechanisms of irradiation creep in graphite material is required to correctly interpret experimental data, explain micromechanical modeling results, and predict whole-core behavior. This project will focus on experimental microscopic data to demonstrate the mechanism of irradiation creep. High-resolution transmission electron microscopy should be able to image both the dislocations in graphite and the irradiation-induced interstitial clusters that pin those dislocations. The team will first prepare and characterize nanoscale samples of virgin nuclear graphite in a transmission electron microscope. Additional samples will be irradiated to varying degrees at the Advanced Test Reactor (ATR) facility and similarly characterized. Researchers will record microstructures and crystal defects and suggest a mechanism for irradiation creep based on the results. In addition, the purchase of a tensile holder for a transmission electron microscope will allow, for the first time, in situ observation of creep behavior on the microstructure and crystallographic defects.
A model system was used to simulate the properties of tribofilms which form during automotive braking. The model system was prepared by ball milling of a blend of 70 vol.% iron oxides, 15 vol.% molybdenum disulfide and 15 vol.% graphite. The resulting mixture was characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and various transmission electron microscopic (TEM) methods, including energy dispersive X-ray spectroscopy (EDXS), high resolution investigations (HRTEM) with corresponding simulation of the HRTEM images, diffraction methods such as scanning nano-beam electron diffraction (SNBED) and selected area electron diffraction (SAED). It could be shown that the ball milling caused a reduction of the grain size of the initial components to the nanometer range. Sometimes even amorphization or partial break-down of the crystal structure was observed for MoS{sub 2} and graphite. Moreover, chemical reactions lead to a formation of surface coverings of the nanoparticles by amorphous material, molybdenum oxides, and iron sulfates as derived from XPS. - Highlights: • Ball milling of iron oxides, MoS{sub 2}, and graphite to simulate a tribofilm • Increasing coefficient of friction after ball milling of the model blend • Drastically change of the diffraction pattern of the powder mixture • TEM & XPS showed the components of the milled mixture and the process during milling. • MoS{sub 2} and graphite suffered a loss in translation symmetry or became amorphous.
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The contributions of individual resin components to total resin weight loss in 600 F air aged Celion 6000/PMR-15 polyimide composites were determined from the overall resin weight loss in the composite by chemically separating the PMR-15 matrix resin into its monomeric components. The individual resin components were also analyzed by spectroscopic techniques in order to elucidate curing and degradation mechanisms of the PMR-15 matrix resin. The isothermal weight loss of the individual resin components during prolonged 600 F thermo-oxidative aging of the composite was correlated to the changes observed in the Fourier Transform infrared spectra and Fourier Transform nuclear magnetic resonance spectra of the individual resin components. The correlation was used to identify the molecular site of the thermo-oxidative changes in PMR-15 polyimide matrix resin during 600 F curing the prolonged 600 F thermo-oxidative aging.
Exposure of graphite targets to high intensity proton beams at neutrino production facilities causes changes in the target material that can result in a shortened operation lifetime. The dominant factors in this process are currently thought to be mechanical in nature resulting primarily from microstructural effects that lead to thermal and structural changes in bulk material properties. As currently planned beam facilities with increased proton energy and intensity begin to come online it will be important to thoroughly understand these processes, and ideally to be able to predict the effects of new beam designs on target properties. Direct analysis of targets exposed to existing high-energy proton beams is complicated by several factors, such as very limited access to proton beam facilities, high associated costs, irradiation times on the order of months, and the resulting radioactivity of irradiated samples that requires special facilities for post-irradiation examination. Much of the existing literature concerning irradiation damage in graphite has been focused on the needs of the nuclear engineering community, however high-energy proton targets operate in a much different environment. In comparison to graphite irradiated in a nuclear reactor, graphite used in proton beam targets receives a higher dose rate, have greater gas production, and experience short irradiation pulses as opposed to continuous irradiation. Low-energy ion irradiation offers a method of inducing similar levels of radiation damage to high-energy protons while avoiding many of the difficulties and limitations associated with high-energy proton beams and the corresponding activated specimen testing. My research described in this thesis focused on investigating how low-energy ion irradiation could be used to induce the same or similar types of microstructural alteration and mechanical property degradation as that seen in high-energy neutrino production target graphites by varying damage le vels and irradiation temperatures prior to post-irradiation characterisation.
When using scanning tunneling microscopy, we characterize a surface carbide that forms such that Dy is deposited on the basal plane of graphite. In order to form carbide islands on terraces, Dy is first deposited at 650–800 K, which forms large metallic islands. Upon annealing at 1000 K, these clusters convert to carbide. Deposition directly at 1000 K is ineffective because nucleation on terraces is inhibited. Reaction is signaled by the fact that each carbide cluster is partially or totally surrounded by an etch pit. The etch pit is one carbon layer deep for most carbide clusters. Carbide clusters are also identifiable by striations on their surfaces. Based on mass balance, and assuming that only the surface layer of carbon is involved in the reaction, the carbide has stoichiometry D y 2 C . This is Dy-rich compared with the most common bulk carbide Dy C 2 , which may reflect limited surface carbon transport to the carbide.
This paper describes the development of input properties for a continuum damage mechanics based material model, Mat 58, within LS-DYNA(Registered Trademark) to simulate the response of a graphite-Kevlar(Registered Trademark) hybrid plain weave fabric. A limited set of material characterization tests were performed on the hybrid graphite-Kevlar(Registered Trademark) fabric. Simple finite element models were executed in LS-DYNA(Registered Trademark) to simulate the material characterization tests and to verify the Mat 58 material model. Once verified, the Mat 58 model was used in finite element models of two composite energy absorbers: a conical-shaped design, designated the "conusoid," fabricated of four layers of hybrid graphite-Kevlar(Registered Trademark) fabric; and, a sinusoidal-shaped foam sandwich design, designated the "sinusoid," fabricated of the same hybrid fabric face sheets with a foam core. Dynamic crush tests were performed on components of the two energy absorbers, which were designed to limit average vertical accelerations to 25- to 40-g, to minimize peak crush loads, and to generate relatively long crush stroke values under dynamic loading conditions. Finite element models of the two energy absorbers utilized the Mat 58 model that had been verified through material characterization testing. Excellent predictions of the dynamic crushing response were obtained.