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NASA NTRS1972

The ablation of graphitic materials in the sublimation regime.

A large variety of graphitic materials have been tested in an arc heated air stream at a surface pressure of 4.3 atm and a nominal surface temperature of 3925 K. Included were commercial and developmental grades of artificial graphites, both two and three dimensional carbon-carbon composites, composites seeded with refractory compounds, and several special materials such as pyrolytic graphite, mesophase graphite, glassy carbon, and natural graphite. ATJ graphite was used as a control material. Except for the seeded materials which had poor performance, the mass loss rate for all the man-made graphitic materials fell within the range of 17 per cent less to 30 per cent more than the rate for ATJ. Thus it is concluded that wide variations in constituents, processing, fabrication and structure have relatively little effect on the ablation performance of graphitic materials, at least under the conditions of the present tests. Particulate mass loss was observed for all the materials tested and is the dominant mechanism for mass removal at the present test conditions. It is suggested that this mechanism results from physical failure, primarily by compressive thermal stress.

Lundell, J. H.↗

NASA NTRS1981

Dynamics of solid dispersions in oil during the lubrication of point contacts. Part 1: Graphite

A Hertzian contact was lubricated with dispersed graphite in mineral oils under boundary lubrication conditions. The contact was optically observed under pure rolling, combined rolling and sliding, and pure sliding conditions. The contact was formed with a steel ball on the flat surface of a glass disk. Photomicrographs are presented which show the distribution of the graphite in and around the contact. Friction and surface damage are also shown for conditions when the base oils are used alone and when graphite is added to the base oils. Under pure rolling and combined rolling and sliding conditions, it is found that, for low speeds, a graphite film can form which will separate the contacting surfaces. Under pure sliding conditions, graphite accumulates at the inlet and sweeps around the contact, but very little of the graphite passes through the contact. The accumulated graphite appears to act as a barrier which reduces the supply of oil available to the contact for boundary lubrication. Friction data show no clear short term beneficial or detrimental effect caused by addition of graphite to the base oil. However, during pure sliding, more abrasion occurs on the polished balls lubricated with the dispersion than on those lubricated with the base oil alone. All observations were for the special case of a highly-polished ball on a glass surface and may not be applicable to other geometries and materials, or to rougher surfaces.

Cusano, C.↗

NASA NTRS1985

Meteoritic evidence that graphite is rare in the interstellar medium

Carbonaceous material from several distinct astrophysical environments that has been identified in primitive meteorites is discussed. Most of this material is not well crystallized graphite, but ranges from kerogenlike macromolecular organic matter to poorly graphitized carbon. Of the small fraction of the carbonaceous material which is graphite, most may have resulted from the graphitization of macromolecular precursors in the solar nebula. Since graphite is more stable than those precursors, preexisting interstellar graphite should have survived in meteorites to at least the same extent as did other forms of carbon. It is concluded from this dearth of graphite that graphitic carbon was not a major component of the interstellar dust at the time of the formation of the solar system.

Nuth, J. A.↗

NASA NTRS1975

Friction and wear of carbon-graphite materials for high energy brakes

Caliper-type brakes simulation experiments were conducted on seven different carbon-graphite material formulations against a steel disk material and against a carbon-graphite disk material. The effects of binder level, boron carbide (B4C) additions, graphite fiber additions, and graphite cloth reinforcement on friction and wear behavior were investigated. Reductions in binder level and additions of B4C each resulted in increased wear. The wear rate was not affected by the addition of graphite fibers. Transition to severe wear and high friction was observed in the case of graphite-cloth-reinforced carbon sliding against a disk of similar composition. This transition was related to the disruption of a continuous graphite shear film that must form on the sliding surfaces if low wear is to occur. The exposure of the fiber structure of the cloth constituent is believed to play a role in the shear film disruption.

Bill, R. C.↗

NASA NTRS1978

Friction and wear of carbon-graphite materials for high-energy brakes

Caliper type brake simulation experiments were conducted on seven different carbon graphite materials formulations against a steel disk material and against a carbon graphite disk material. The effects of binder level, boron carbide (B4C) additions, SiC additions, graphite fiber additions, and graphite cloth reinforcement on friction and wear behavior were investigated. Reductions in binder level, additions of B4C, and additions of SiC each resulted in increased wear. The wear rate was not affected by the addition of graphite fibers. Transition to severe wear and high friction was observed in the case of graphite-cloth-reinforced carbon sliding against a disk of similar composition. The transition was related to the disruption of a continuous graphite shear film that must form on the sliding surfaces if low wear is to occur.

Bill, R. C.↗

NASA NTRS1987

Design, fabrication and performance of small, graphite electrode, multistage depressed collectors with 200-W, CW, 8- to 18-GHz traveling-wave tubes

Small multistage depressed collectors (MDC's) which used pyrolytic graphite, ion-beam-textured pyrolytic graphite, and isotropic graphite electrodes were designed, fabricated, and evaluated in conjuntion with 200-W, continuous wave (CW), 8- to 18-GHz traveling-wave tubes (TWT's). The design, construction, and performance of the MDC's are described. The bakeout performance of the collectors, in terms of gas evolution, was indistinguishable from that of typical production tubes with copper collectors. However, preliminary results indicate that some additional radiofrequency (RF) and dc beam processing time (and/or longer or higher temperature bakeouts) may be needed beyond that of typical copper electrode collectors. This is particularly true for pyrolytic graphite electrodes and for TWT's without appendage ion pumps. Extended testing indicated good long-term stability of the textured pyrolytic graphite and isotropic graphite electrode surfaces. The isotropic graphite in particular showed considerable promise as an MDC electrode material because of its high purity, low cost, simple construction, potential for very compact overall size, and relatively low secondary electron emission yield characteristics in the as-machined state. However, considerably more testing experience is required before definitive conclusions on its suitability for electronic countermeasure systems and space TWT's can be made.

Ebihara, Ben T.↗

NASA NTRS1987

Effects of sequential treatment with fluorine and bromine on graphite fibers

Three pitch based graphite fibers with different degrees of graphitization and one polyacryonitrile (PAN) based carbon fiber from Amoco Corporation were treated with 1 atm, room temperature fluorine gas for 90 hrs. Fluorination resulted in higher electrical conductivity for all pitch fibers. Further bromination after ambient condition defluorination resulted in further increases in electrical defluorination conductivity for less graphitized, less structurally ordered pitch fibers (P-55) which contain about 3% fluorine by weight before bromination. This product can be stable in 200 C air, or 100% humidity at 60 C. Due to its low cost, this less graphitized fiber may be useful for industrial application, such as airfoil deicer materials. The same bromination process, however, resulted in conductivity decreases for fluorine rich, more graphitized, structurally oriented pitch fibers (P-100 and P-75). Such decreases in electrical conductivity were partially reversed by heating the fibers at 185 C in air. Differential scanning calorimetric (DSC) data indicated that the more graphitized fibers (P-100) contained BrF3, whereas the less graphitized fibers (P-55) did not.

Hung, Ching-Cheh↗

NASA NTRS1994

Formation and chemical reactivity of carbon fibers prepared by defluorination of graphite fluoride

Defluorination of graphite fluoride (CFX) by heating to temperatures of 250 to 450 C in chemically reactive environments was studied. This is a new and possibly inexpensive process to produce new carbon-based materials. For example, CF 0.68 fibers, made from P-100 carbon fibers, can be defluorinated in BrH2C-CH = CH-CH2Br (1,4-dibromo-2butene) heated to 370 C, and graphitized to produce fibers with an unusually high modulus and a graphite layer structure that is healed and cross-linked. Conversely, a sulfur-doped, visibly soft carbon fiber was produced by defluorinating CF 0.9 fibers, made from P-25, in sulfur (S) vapor at 370 C and then heating to 660 C in nitrogen (N2). Furthermore, defluorination of the CF 0.68 fibers in bromine (Br2) produced fragile, structurally damaged carbon fibers. Heating these fragile fibers to 1100 C in N2 caused further structural damage, whereas heating to 150 C in bromoform (CHBr3) and then to 1100 C in N2 healed the structural defects. The defluorination product of CFX, tentatively called activated graphite, has the composition and molecular structure of graphite, but is chemically more reactive. Activated graphite is a scavenger of manganese (Mn), and can be intercalated with magnesium (Mg). Also, it can easily collect large amounts of an alloy made from copper (Cu) and type 304 stainless steel to form a composite. Finally, there are indications that activated graphite can wet metals or ceramics, thereby forming stronger composites with them than the pristine carbon fibers can form.

Hung, Ching-Cheh↗

NASA NTRS1977

Research on Graphite Reinforced Glass Matrix Composites

This report contains the results obtained in the first twelve months of research under NASA Langley Contract NAS1-14346 for the origination of graphite-fiber reinforced glass matrix composites. Included in the report is a summary of the research by other investigators in this area. The method selected to form the composites consisted of pulling the graphite fiber through a slurry containing powdered glass, winding up the graphite fiber and the glass it picks up on a drum, drying, cutting into segments, loading the tape segment into a graphite die, and hot pressing. During the course of the work, composites were made with a variety of graphite fibers in a C.G.W. 7740 (Pyrex) glass matrix. The graphite fibers used included Hercules HMS, Hercules HTS, Thornel 300S, and Celanese DG-102 and, of these, the Hercules HMS and Celanese DG-102 graphite fibers in C.G.W. 7740 gave the most interesting but widely different results. Hercules HMS fiber in C.G.W. 7740 glass (Pyrex) showed an average four-point flexural strength of 848 MPa or 127,300 psi. As the test temperature was raised from room temperature to 560 C in argon or vacuum, the strength was higher by 50 percent. However, in air, similar tests at 560 C gave a severe loss in strength. These composites also have good thermal cycle properties in argon or vacuum, greatly increased toughness compared to glass, and no loss in strength in a 100 cycle fatigue test. Celanese DG-102 fiber in C.G.W. 7740 glass (Pyrex) had a much lower flexural strength but did not suffer any loss in this strength when samples were heated to 560 C in air for 4 hrs.

Bacon, J. F.↗

NASA NTRS2000

Heat Transfer Performances of Pool Boiling on Metal-Graphite Composite Surfaces

Nucleate boiling, especially near the critical heat flux (CHF), can provide excellent economy along with high efficiency of heat transfer. However, the performance of nucleate boiling may deteriorate in a reduced gravity environment and the nucleate boiling usually has a potentially dangerous characteristic in CHF regime. That is, any slight overload can result in burnout of the boiling surface because the heat transfer will suddenly move into the film-boiling regime. Therefore, enhancement of nucleate boiling heat transfer becomes more important in reduced gravity environments. Enhancing nucleate boiling and critical heat flux can be reached using micro-configured metal-graphite composites as the boiling surface. Thermocapillary force induced by temperature difference between the graphite-fiber tips and the metal matrix, which is independent of gravity, will play an important role in bubble detachment. Thus boiling heat transfer performance does not deteriorate in a reduced-gravity environment. Based on the existing experimental data, and a two-tier theoretical model, correlation formulas are derived for nucleate boiling on the copper-graphite and aluminum-graphite composite surfaces, in both the isolated and coalesced bubble regimes. Experimental studies were performed on nucleate pool boiling of pentane on cooper-graphite (Cu-Gr) and aluminum-graphite (Al-Gr) composite surfaces with various fiber volume concentrations for heat fluxes up to 35 W per square centimeter. It is revealed that a significant enhancement in boiling heat transfer performance on the composite surfaces is achieved, due to the presence of micro-graphite fibers embedded in the matrix. The onset of nucleate boiling (the isolated bubble regime) occurs at wall superheat of about 10 C for the Cu-Gr surface and 15 C for the Al-Gr surface, much lower than their respective pure metal surfaces. Transition from an isolated bubble regime to a coalesced bubble regime in boiling occurs at a superheat of about 14 C on Cu-Gr surface and 19 C on Al-Gr surface.

Zhang, Nengli↗

NASA NTRS2004

The Use of Pristine and Intercalated Graphite Fiber Composites as Buss Bars in Lead-Acid Batteries

This study was conducted as a part of the Firefly Energy Space Act Agreement project to investigate the possible use of composite materials in lead acid batteries. Specifically, it examined the use of intercalated graphite composites as buss bars. Currently, buss bars of these batteries are made of lead, a material that is problematic for several reasons. Over time, the lead is subject to both corrosion at the positive plate and sulfation at the negative plate, resulting in decreased battery life. In addition, the weight and size of the lead buss bars make for a heavy and cumbersome battery that is undesirable. Functionality and practicality of lead buss bars is adequate at best; consequently, investigation of more efficient composite materials would be advantageous. Practically speaking, graphite composites have a low density that is nearly one fourth that of its lead counterpart. A battery made of less dense materials would be more attractive to the consumer and the producer because it would be light and convenient. More importantly, low weight would be especially beneficial because it would result in greater overall power density of the battery. In addition to power density, use of graphite composite materials can also increase the life of the battery. From a functional standpoint, corrosion and sulfation at the positive and negative plates are major obstacles when considering how to extend battery life. Neither of these reactions are a factor when graphite composites replace lead parts because graphite is chemically non-reactive with the electrolyte within the battery. Without the problem of corrosion or sulfation, battery life expectancy can be almost doubled. The replacement of lead battery parts with composite materials is also more environmentally favorable because of easy disposal of organic materials. For this study, both pristine and bromine intercalated single-ply graphite fiber composites were created. The composites were fabricated in such a way as to facilitate their use in a 3" x 1/2" buss bar test cell. The prime objective of this investigation was to examine the effectiveness of a variety of graphite composite materials to act as buss bars and carry the current to and from the positive and negative battery plates. This energy transfer can be maximized by use of materials with high conductivity to minimize the buss resistance. Electrical conductivity of composites was measured using both a contactless eddy current probe and a four point measurement. In addition, the stability of these materials at battery-use conditions was characterized.

Opaluch, Amanda M.↗

NASA NTRS2011

Stable dispersions of polymer-coated graphitic nanoplatelets

A method of making a dispersion of reduced graphite oxide nanoplatelets involves providing a dispersion of graphite oxide nanoplatelets and reducing the graphite oxide nanoplatelets in the dispersion in the presence of a reducing agent and a polymer. The reduced graphite oxide nanoplatelets are reduced to an extent to provide a higher C/O ratio than graphite oxide. A stable dispersion having polymer-treated reduced graphite oxide nanoplatelets dispersed in a dispersing medium, such as water or organic liquid is provided. The polymer-treated, reduced graphite oxide nanoplatelets can be distributed in a polymer matrix to provide a composite material.

Stankovich, Sasha↗

NASA NTRS1956

Energy of Cohesion, Compressibility, and the Potential Energy Functions of the Graphite System

The lattice summations of the potential energy of importance in the graphite system have been computed by direct summation assuming a Lennard‐Jones 6–12 potential between carbon atoms. From these summations, potential energy curves were constructed for interactions between a carbon atom and a graphite monolayer, between a carbon atom and a graphite surface, between a graphite monolayer and a semi‐infinite graphite crystal and between two graphite semi‐infinite crystals. Using these curves, the equilibrium distance between two isolated physically interacting carbon atoms was found to be 2.70 a, where a is the carbon‐carbon distance in a graphite sheet. The distance between a surface plane and the rest of the crystal was found to be 1.7% greater than the interlayer spacing. Theoretical values of the energy of cohesion and the compressibility were calculated from the potential curve for the interaction between two semi‐infinite crystals. They were ΔE c = —330 ergs/cm 2 and β = 3.18×10 —12 cm 2 /dyne, respectively. These compared favorably with the experimental values of ΔE c = —260 ergs/cm 2 and β = 2.97×10 —2 cm 2 /dyne.

L A Girifalco↗

NASA NTRS2021

Tunable Pseudocapacitive Intercalation of Chloroaluminate Anions into Graphite Electrodes for Rechargeable Aluminum Batteries

Rechargeable aluminum-graphite batteries using chloroaluminate-containing electrolytes have been the focus of significant research, particularly due to their high-rate capabilities. Engineered graphite electrodes have been shown to exhibit supercapacitor-like rate performance, despite the fact they store charge via the electrochemical intercalation of polyatomic AlCl4− anions. However, the origins of such rate capabilities are not well understood. Here, using electrochemical techniques, we disentangle quantitatively the diffusion-limited Faradaic, pseudocapacitive, and capacitive contributions to charge storage, revealing that AlCl4− anions intercalate into graphite with significant pseudocapacitive characteristics due to low ion diffusion limitations. Pristine and mildly exfoliated graphites are compared, where exfoliation resulted in significantly higher pseudocapacitive AlCl4− intercalation at the highest potential redox pair as well as higher galvanostatic capacity retention at faster discharge rates. The relationships between graphite structure, ion mass transport, and the overall rate of electrochemical AlCl4− intercalation are discussed. Ion diffusion within the electrolyte phase of the porous electrode is shown to play a key role in controlling the rate of intercalation at higher potentials and faster rates, which can be enhanced by reducing electrode tortuosity. The results establish that chloroaluminate anion intercalation into graphite exhibits non-diffusion-limited pseudocapacitive contributions that are tunable by modifying the graphite structure.

Jeffrey H. Xu↗

NASA NTRS1972

Adsorption of carbon monoxide and hydrogen on graphite.

Adsorption of carbon monoxide and hydrogen was investigated on three graphites: a high-density pyrolytic graphite, a small-grain extruded graphite, and a processed pyrolytic graphite tape. The sticking probability of CO was found to decrease rapidly as the average surface coverage approached 0.01 monolayer. Lower sticking probabilities were observed on the highly oriented pyrolytic graphite which indicated that adsorption occurs principally on the edge atoms. There is negligible adsorption of molecular hydrogen on graphite that has been heated to 2400 K in vacuo.

Beitel, G. A.↗

NASA NTRS1974

The action of macrosounds on graphite ore and derived products

A suspension of graphite ore, floated graphite, and the gangue left over from flotation were subjected to the action of macrosounds under determinant conditions. The following was found: (1) The graphite ore undergoes an efficient settling action. (2) The floated graphite is strongly crushed down to the dimensions of colloidal graphite. (3) The gangue left over from flotation can be further processed to recuperate graphite from its nuclei.

Bradeteanu, C.↗

NASA NTRS1975

Friction and wear of metals in contact with pyrolytic graphite

Sliding friction experiments were conducted with gold, iron, and tantalum single crystals sliding on prismatic and basal orientations of pyrolytic graphite in various environments, including vacuum, oxygen, water vapor, nitrogen, and hydrogen bromide. Surfaces were examined in the clean state and with various adsorbates present on the graphite surfaces. Auger and LEED spectroscopy, SEM, and EDXA were used to characterize the graphite surfaces. Results indicate that the prismatic and basal orientations do not contain nor do they chemisorb oxygen, water vapor, acetylene, or hydrogen bromide. All three metals exhibited higher friction on the prismatic than on the basal orientation and these metals transferred to the atomically clean prismatic orientation of pyrolytic graphite. No metal transfer to the graphite was observed in the presence of adsorbates at 760 torr. Ion bombardment of the graphite surface with nitrogen ions resulted in the adherence of nitrogen to the surface.

Buckley, D. H.↗

NASA NTRS1976

Graphite and ablative material response to CO2 laser, carbon-arc, and xenon-arc radiation

The behavior was investigated of graphite and several charring ablators in a variety of high-radiative heat-flux environments. A commercial-grade graphite and nine state-of-the-art charring ablators were subjected to various radiative environments produced by a CO2 laser and a carbon arc. Graphite was also tested in xenon-arc radiation. Heat-flux levels ranged from 10 to 47 MW/sq m. Tests were conducted in air, nitrogen, helium, and a CO2-N2 mixture which simulated the Venus atmosphere. The experimental results were compared with theoretical results obtained with a one-dimensional charring-ablator analysis and a two-dimensional subliming-ablator analysis. Neither the graphite nor the charring ablators showed significant differences in appearance or microstructure after testing in the different radiative environments. The performance of phenolic nylon and graphite was predicted satisfactorily with existing analyses and published material property data. Good agreement between experimental and analytical results was obtained by using sublimation parameters from a chemical nonequilibrium analysis of graphite sublimation. Some charring ablators performed reasonably well and could withstand radiative fluxes of the level encountered in certain planetary entries. Other materials showed excessive surface recession and/or large amounts of cracking and spalling, and appear to be unsuitable for severe radiative environments.

Brewer, W. D.↗