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At least 19 records

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

Compression behavior of graphite-thermoplastic and graphite-epoxy panels with circular holes or impact damage

An experimental investigation of the compression behavior of laminated specimens made from graphite-epoxy tape, graphite-thermoplastic tape and graphite-thermoplastic fabric was conducted. Specimens with five different stacking sequences were loaded to failure in uniaxial compression. Some of the specimens had central circular holes with diameters up to 65 percent of the specimen width. Other specimens were subjected to low speed impact with impact energies up to 35 J prior to compressive loading. This investigation indicates that graphite-thermoplastic specimens with holes have up to 15 percent lower failure stresses and strains than graphite-epoxy specimens with the same stacking sequence and hole size. However, graphite-thermoplastic specimens subjected to low speed impact have up to 15 percent higher failure stresses and strains than graphite-epoxy specimens with the same stacking sequence and impact energy. Compression tests of graphite-thermoplastic specimens constructed of unidirectional tape and fabric indicate that the material form has little effect on failure strains in specimens with holes or low speed impact damage.

Jegley, Dawn C.

Compression behavior of graphite-epoxy and graphite-thermoplastic panels with circular holes or impact damage

An experimental investigation of the compression behavior of laminated specimens made from graphite-epoxy tape (AS4-3502), graphite-thermoplastic tape (AS4-PEEK), and graphite-thermoplastic fabric (AS4-PEEK) was conducted. Specimens with five different stacking sequences were loaded to failure in uniaxial compression. Some of the specimens had central circular holes with diameters up to 65 percent of the specimen width. Other specimens were subjected to low speed impact with impact energy up to 30 J prior to compressive loading. This investigation indicates that graphite-thermoplastic specimens with holes have up to 15 percent lower failure stresses and strains than graphite-epoxy specimens with the same stacking sequence and hole size. However, graphite-thermoplastic specimens subjected to low speed impact have up to 15 percent higher failure stresses and strains than graphite-epoxy specimens with the same stacking sequence and impact energy. Compression tests of graphite-thermoplastic specimens constructed of unidirectional tape and of fabric indicate that the material form has little effect on failure strains in specimens with holes or low speed impact damage.

Jegley, Dawn C.

Evaluation of long-duration exposure to the natural space environment on graphite-polyimide and graphite-epoxy mechanical properties (A0175)

The primary objective of this experiment is to accumulate the needed operational data associated with the exposure of graphite-polyimide and graphite-epoxy material to the environments of space. The experiment will be mounted in two 3-in.-deep peripheral trays. Graphite-polyimide specimens will occupy 1 1/3 trays and the graphite-epoxy specimens will occupy two-thirds of a tray. The experiment approach requires two matched sets of specimens with traceable records that are maintained for materials processing and specimen quality. After fabrication, one set of each test specimen will be sectioned and structurally tested to serve as a data baseline. After the flight, the other set of specimens will undergo extensive measurements of mechanical properties for comparison with the original data baseline. Structural testing of the graphite-polyimide specimens will provide strength and elastic data in tension, compression, and shear. Transverse tension microcracking and crack propagation will be evaluated by photomicroscopy. Structural testing of the graphite-epoxy specimens will include verification of laminate, core, adhesive, and fatigue properties as applied to the design and analysis of the payload bay door. Microcracking and crack propagation will also be analyzed by photomicroscopy.

Powell, J. H.

Ferric chloride graphite intercalation compounds prepared from graphite fluoride

The reaction between graphite fluoride and ferric chloride was observed in the temperature range of 300 to 400 C. The graphite fluorides used for this reaction have an sp3 electronic structure and are electrical insulators. They can be made by fluorinating either carbon fibers or powder having various degrees of graphitization. Reaction is fast and spontaneous and can occur in the presence of air. The ferric chloride does not have to be predried. The products have an sp2 electronic structure and are electrical conductors. They contain first stage FeCl3 intercalated graphite. Some of the products contain FeCl2*2H2O, others contain FeF3 in concentrations that depend on the intercalation condition. The graphite intercalated compounds (GIC) deintercalated slowly in air at room temperature, but deintercalated quickly and completely at 370 C. Deintercalation is accompanied by the disappearing of iron halides and the formation of rust (hematite) distributed unevenly on the fiber surface. When heated to 400 C in pure N2 (99.99 vol %), this new GIC deintercalates without losing its molecular structure. However, when the compounds are heated to 800 C in quartz tube, they lost most of its halogen atoms and formed iron oxides (other than hematite), distributed evenly in or on the fiber. This iron-oxide-covered fiber may be useful in making carbon-fiber/ceramic-matrix composites with strong bonding at the fiber-ceramic interface.

Hung, Ching-Cheh

Ferrix Chloride-Graphite Intercalation Compounds Prepared From Graphite Flouride

The reaction between graphite fluoride and ferric chloride was observed in the temperature range of 300 to 400 C. The graphite fluorides used for this reaction have an sp(sup 3) electronic structure and are electrical insulators. They can be made by fluorinating either carbon fibers or powder having various degrees of graphitization. Reaction is fast and spontaneous and can occur in the presence of air. The ferric chloride does not have to be predried. The products have an sp(sup 2) electronic structure and are electrical conductors. They contain first-stage FeCl3 intercalated graphite. Some of the products contain FeCl2 (center dot) 2H2O, others contain FeF3, in concentrations that depend on the intercalation condition. The graphite intercalated compounds (GIC) deintercalated slowly in air at room temperature, but deintercalated quickly and completely at 370 C. Deintercalation is accompanied by the disappearance of iron halides and the formation of rust (hematite) distributed unevenly on the fiber surface. When heated to 400 C in pure N2 (99.99 vol%), this new GIC deintercalates without losing its molecular structure. However, when the compounds are exposed to 800 C N2, in a quartz tube, they lost most of their halogen atoms and formed iron oxides (other than hematite), distributed evenly in or on the fiber.

Hung, Ching-Cheh

Graphite Oxidation Rate Study on ET-10 and ETU-10 Grades - Task 4: QA Support and Testing for Structural Graphite Oxidation

INL performed targeted oxidation tests to measure oxidation rates for samples of ET-10 and ETU-10 graphite under CRADA No. 21CRA22 Mod. 3, Annex A, “Tritium Testing to Support Kairos Power Advanced Reactor Demonstration” (04/02/2024). All testing was conducted within INL’s Carbon Characterization Laboratory (CCL) using test standard ASTM D7542-21 "Standard Test Method for Air Oxidation of Carbon and Graphite in the Kinetic Regime" [ASTM International, 2021]. Kairos Power provided all test specimens through its graphite vendor Ibiden, Inc. to INL and ASTM specimen specified dimensions. Information within this report only provides the Arrhenius oxidation rate plots as a function of temperature for each graphite grade tested. The raw mass loss per time data will be provided on the Nuclear Data Management and Analysis System (NDMAS) portal located on the INL information system.

36 MATERIALS SCIENCE

Polyfunctional epoxies. I - Rubber-toughened brominated and nonbrominated formulations for graphite composites. II - Nonrubber versus rubber-toughened brominated formulations for graphite composites

A new trifunctional epoxy resin, Tris-(hydroxyphenyl) methane triglycidyl ether, is compared to a state-of-the-art tetraglycidyl 4,4'-diaminodiphenyl methane (TGDDM), in graphite composites. Rubber-toughened brominated formulations of the epoxy resin are compared to nonbrominated ones in terms of their mechanical performance, environmental stability, thermochemical behavior, and flame retardancy. It is shown that the new resin performs almost the same way as the TGDDM does, but has improved glass transition temperature and environmental properties. Brominated polymeric additives (BPA) of different molecular weights are tested as a Br source to flame retardant graphite epoxy composites. The optimal molecular weight of the BPA and its polymeric backbone length are derived and compared with a 10 percent rubber-toughened formulation of the epoxy resin. Results indicate that when the Br content in the graphite composite is increased without the use of rubber, the mechanical properties improved. The use of BPAs as tougheners for graphite composites is also considered.

Nir, Z.

Investigation of Ceramic, Graphite, and Chrome-plated Graphite Nozzles on Rocket Engine

The use of ceramic material for rocket nozzles and the effectiveness of preventing oxidation and erosion of graphite nozzles by chrome-plating the internal surface were investigated. A supported ceramic nozzle, cracked by initial operation, was operated a second time without further cracking or damage. Chrome-plating the internal surface of graphite nozzles effectively prevented oxidation and erosion that occurred during operation with unprotected graphite.

CERAMICS

On the Efficacy of Repeat Voltage Holds for Conditioning and Calendar Life Testing of Graphite and Silicon Cells

Voltage-hold (V-hold) protocols have shown promise toward calendar lifetime analysis of cells with graphite (Gr) and silicon (Si) anodes. In this work, repeat V-holds are performed on Gr and Si cells paired with lithium iron phosphate cathodes to delineate their beneficial role in formation and conditioning. We find that V-hold at the top of charge supplements constant current cycling in conditioning the cell to higher capacities for both Gr and Si cells after the first V-hold. A reduced order model provides the irreversible capacity proportions of each V-hold. With each repeat V-hold, parasitic loss of lithium to the solid electrolyte interphase (SEI) decreases on both Gr and Si cells. Gr cells show the square-root-of-time capacity loss behavior within 200 h of V-hold, indicative of its fast relaxation and low impact of reference performance test cycles on the SEI growth. Lifetime estimates from repeat V-holds on Gr can reach years. Si exhibits longer transition times from kinetic to diffusion-limited SEI growth, evidenced by the 400 h and 200 h holds showing square-root-of-time and linear behavior, respectively. Lifetime predictions from repeat V-holds on Si only reach 1–2 months, highlighting its limitations. Recommended duration of V-holds for Si cells should be ≥400 h.

25 ENERGY STORAGE

Fabrication and physical testing of graphite composite panels utilizing woven graphite fabric with current and advanced state-of-the-art resin systems

Three weaves were evaluated; a balanced plain weave, a balanced 8-harness satin weave, and a semiunidirectional crowfoot satin weave. The current state-of-the-art resin system selected was Fiberite's 934 Epoxy; the advanced resin systems evaluated were Phenolic, Phenolic/Novolac, Benzyl and Bismaleimide. The panels were fabricated for testing on NASA/Ames Research Center's Composites Modification Program. Room temperature mechanical tests only were performed by Hitco; the results are presented.

Lee, S. C. S.

Notched graphite polymimide composites at room and notched graphite polymide composites at room and elevated temperatures

The fracture behavior in graphite/polyimide (Gr/PI) Celion 6000/PMR-15 composites was characterized. Emphasis was placed on the correlation between the observed failure modes and the deformation characteristics of center-notched Gr/Pl laminates. Crack tip damage growth, fracture strength and notch sensitivity, and the associated characterization methods were also examined. Special attention was given to nondestructive evaluation of internal damage and damage growth, techniques such as acoustic emission, X-ray radiography, and ultrasonic C-scan. Microstructural studies using scanning electron microscopy, photomicrography, and the pulsed nuclear magnetic resonance technique were employed as well. All experimental procedures and techniques are described and a summary of representative results for Gr/Pl laminates is given.

Awerbuch, J.

Evaluation of long-duration exposure to the natural space environment on graphite-polyimide and graphite-epoxy mechanical properties

Experiment AO175 involved passive exposure (on oblique leading and trailing faces of LDEF) of carbon-fiber reinforced laminates of epoxy, bismaleimide, and polyimide resins. Post-flight evaluation included: optical examination of exposed surfaces, panel weight and distortion measurements, ultrasonic c-scan inspection, and conventional mechanical testing of coupons machined from the panel.

Vyhnal, Richard F.