SEARCH · Search NASA

Results for “Intercalation”

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.

SourceResearch connectionFrom yearThrough year

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 19 records

All sources NASA NTRS DOE OSTI

NASA NTRS1993

A method to remove intercalates from bromine and iodine intercalated carbon fibers

Upon exposure to room-temperature fluorine, intercalated carbon fibers (containing either bromine alone or iodine and bromine together) become heavier and less stable. For Amoco P-100 graphitized carbon fibers which were intercalated with 18 percent bromine by weight, 1 hr of fluorine exposure results in a large weight increase, but causes only a small decrease in thermal stability. More than l hr of fluorine exposure time results in small additional increases in fiber weight, but significant further decreases in fiber thermal stability. Such phenomena do not occur if the fluorine exposure is at 250 C. These observations suggest the mechanism that at room temperature, fluorine is absorbed quickly by the intercalated fibers and intercalated slowly into the fibers. Most of the original intercalates are replaced by fluorine in the process of fluorine intercalation. Under an inert environment, the bromine intercalated fibers are much more thermally stable. After 800 C vacuum heating for two weeks, the brominated fibers lost about 45 percent of their bromine, and their resistivity increased from 64 omega-cm to a range of 95 to 170 micro omega-cm. This is still much lower than the 300 micro omega-cm value for pristine P-100. For practical purposes, in order to preserve their thermal stability, brominated fibers need to be protected from exposure to fluorine at room temperature, or to any intercalate at a temperature where, upon direct contact to graphite, an intercalation compound can easily be formed.

Hung, Ching-Cheh↗

NASA NTRS1985

Graphite fiber intercalation: Dynamics of the bromine intercalation process

The resistance of pitch-based graphite fibers was monitored, in situ, during a series of bromine intercalation experiments. The threshold pressure for the bromine intercalation of pitch-based fibers was estimated to be 102 torr. When the bromine atmosphere was removed from the reaction chamber, the resistivity of the intercalated graphite fibers increased consistently. This increase was attributed to loss of bromine from the perimeter of the fiber. The loss was confirmed by mapping the bromine concentration across the diameter of single intercalated fibers with either energy dispersive spectroscopy or scanning Auger microscopy. A statistical study comparing fibers intercalated in bromine vapor with fibers intercalated in bromine liquid showed that similar products were obtained with both methods of intercalation.

Jaworske, D. A.↗

NASA NTRS1986

Graphite fiber intercalation: Basic properties of copper chloride intercalated fibers

In situ resistance measurements were used to follow the intercalation of copper chloride in pitch-based fibers. Subsequent single fiber resistivity measurements reveal a large range of resistivities, from 13 to 160 micro-ohms cm. Additional density measurements reveal a bimodal distribution of mass densities. The dense fibers have lower resistivities and correspond to the stage III compound identified by X-ray diffraction. Neither resistivity nor density correlate with diameter. Both energy dispersive spectroscopy and mass density data suggest that excess chlorine resides in the intercalated fiber, resulting in a stoichiometry of C4.9n CuCl2.5 (where n is the stage number) for the denser fibers. Finally, thermogravimetric analysis shows a 33 percent loss in mass upon heating to 700C. This loss in mass is attributed to loss of both chlorine and carbon.

Jaworske, D. A.↗

NASA NTRS1994

Graphite intercalation compound with iodine as the major intercalate

Halogenated graphite CBr(x)I(y) (I less than y/x less than 10) was made by exposing graphite materials to either pure Br2 or an I2/Br2/HBr mixture to initiate the reaction, and then to iodine vapor containing a small amount of Br2/HBr/IBr to complete the intercalation reaction. Wetting of the graphite materials by the I2/Br2/HBr mixture is needed to start the reaction, and a small amount of Br2/HBr/IBr is needed to complete the charge transfer between iodine and carbon. The interplanar spacings for the graphite materials need to be in the 3.35 to 3.41 A range. The X-ray diffraction data obtained from the halogenated HOPG indicate that the distance between the two carbon layers containing intercalate is 7.25 A. Electrical resistivity of the fiber product is from 3 to 6.5 times the pristine value, The presence of a small amount of isoprene rubber in the reaction significantly increased the iodine-to-bromine ratio in the product. In this reaction, rubber is known to generate HBr and to slowly remove bromine from the vapor. The halogenation generally caused a 22 percent to 25 percent weight increase. The halogens were found uniformly distributed in the product interior. However, although the surface contains very little iodine, it has high concentrations of bromine and oxygen. It is believed that the high concentrations of bromine and oxygen in this surface cause the halogenated fiber to be more resistant to structural damage during subsequent fluorination to fabricate graphite fluoride fibers.

Hung, Ching-Cheh↗

NASA NTRS1992

Graphite intercalation compound with iodine as the major intercalant

Halogenated CBr(sub x)I(sub y) (1 less than y/x less than 10) was made by exposing graphite materials with interplanar spacing in the 3.35 to 3.41 A range to either pure Br2 or an I2-Br2 mixture, and then to iodine vapor containing a small amount of Br2. The electrical resistivity of this product is from 3 to 6.5 times the pristine value. The presence of a small amount of isoprene rubber in the reaction significantly increased the iodine to bromine ratio in the product. In this reaction, rubber is known to generate HBr and to slowly remove bromine from the vapor. The halogenation generally caused a 22 to 25 percent weight increase. The halogens were found uniformly distributed in the product interior. However, although the surface contains very little iodine, it has high concentrations of bromine and oxygen. It is believed that the high concentrations of bromine and oxygen in this surface cause the halogenated fiber to be more resistant to fluorine attack during subsequent fluorination to fabricate graphite fluoride fibers.

Hung, Ching-Cheh↗

NASA NTRS1995

Room-Temperature Fluorine-Induced Decrease in the Stability of Bromine and Iodine Intercalated Carbon Fibers

Upon exposure to room-temperature fluorine, intercalated carbon fibers (containing either bromine alone or iodine and bromine together) become heavier and less stable. For Amoco P-100 graphitized carbon fibers, which were intercalated with 18 wt percent bromine, 1 hour of fluorine exposure resulted in a large weight increase but caused only a small decrease in thermal stability. An additional 89 hours of fluorine exposure time resulted in small additional increases in fiber weight, but significant further decreases in fiber thermal stability. Such phenomena of weight increase and stability decrease do not occur if the intercalated fibers are exposed to 250 C fluorine. These observations suggest that, at room temperature, fluorine is absorbed quickly by the intercalated fibers and is intercalated slowly into the fibers. Most of the original intercalates are replaced by fluorine in the process of fluorine intercalation. In an inert environment, the bromine intercalated fibers are much more thermally stable. After 800 C vacuum heating for 2 weeks, the brominated fibers lost about 45% of their bromine, and their resistivity increased from 64 mu(Omega)-cm to a range of 95-170 mu(Omega)-cm. This is still much lower than the value of 300 mu(Omega)-cm for pristine P-100. For practical purposes, to preserve their thermal stability, brominated fibers need to be protected from exposure to fluorine at room temperature or to any intercalate at a temperature where, upon direct contact with graphite, an intercalation compound can easily be formed.

Hung, Ching-Cheh↗

NASA NTRS1985

Environmental stability of intercalated graphite fibers

Graphite fibers intercalated with bromine, iodine monochloride, ferric chloride, and cupric chloride were subjected to stability tests under four environments which are encountered by engineering materials in the aerospace industry: ambient laboratory conditions, as would be experienced during handling operations and terrestrial applications; high vacuum, as would be experienced in space applications; high humidity, as would be experienced in marine applications; and high temperature, as would be experienced in some processing steps and applications. Monitoring the resistance of the fibers at ambient laboratory conditions revealed that only the ferric chloride intercalated fibers were unstable, due to absorption of water from the air. All four types of intercalated fibers were unstable, due to absorption of water from the air. All four types of intercalated fibers were stable for long periods under high vacuum. Ferric chloride, cupric chloride, and iodine monochloride intercalated fibers were sensitive to high humidity conditions. All intercalated fibers began to degrade above 250 C. The order of their thermal stability, from lowest to highest, was cupric chloride, iodine monochloride, bromine, and ferric chloride. Of the four types of intercalated fibers tested, the bromine intercalated fibers appear to have the most potential for application, based on environmental stability.

Gaier, J. R.↗

NASA NTRS1985

Environmental stability of intercalated graphite fibers

Gaier, J. R.↗

NASA NTRS1984

Dynamics of graphite fiber intercalation: In situ resistivity measurements with a four point probe

The dynamics of ferric chloride intercalation of single graphite fibers were studied, in situ, using a four point dc bridge. Measurements before, during and after the intercalation showed that the intercalation occurred within minutes at 200 C. Changes in fiber resistivity after exposure to air suggested hydration of the graphite intercalation compound. Deintercalation of the ferric chloride was initiated at temperatures in excess of 400 C. cycling the intercalant into and out of the graphite fiber gave no improvements in fiber resistivity. The activation energy of the ferric chloride intercalation reaction was found to be 17 + or - 4 kcal/mol 1 consistent with the concept of a preliminary nucleation step in the intercalation reaction.

Jaworske, D. A.↗

NASA NTRS1998

Fabrication and Resistivity of IBr Intercalated Vapor-Grown Carbon Fiber Composites

Composites using vapor-crown carbon fibers (VGCF), the most conductive of the carbon fiber types, are attractive for applications where low density, high strength, and at least moderate conductivity are required, such as electromagnetic interference shielding covers for spacecraft. The conductivity can be enhanced another order of magnitude by intercalation of the VGCF. If a high Z intercalate is used, the protection of components from ionizing radiation can be enhanced also. Thus, the intercalation of VGCF with IBr is reported. Since composite testing is required to verify properties, the intercalation reaction optimization, stability of the intercalation compound, scale-up of the intercalation reaction, composite fabrication, and resistivity of the resulting composites is also reported. The optimum conditions for low resistivity and uniformity for the scaled up reaction (20-30 g of product) were 114 C for at least 72 hr, yielding a fiber with a resistivity of 8.7+/-2 micro-Omega-cm. The thermal stability of these fibers was poor, with degradation occurring at temperatures as low as 40 C in air, though they were insensitive to water vapor. Composite resistivity was 20-30 micro-Omega-cm, as measured by contactless conductivity measurements, about a factor of five higher than would be expected from a simple rule of mixtures. The addition of 1.0 percent Br2, intercalated microfibers increased the resistivity of the composites by more than 20 percent.

Gaier, James R.↗

NASA NTRS2018

Compositions and Methods Associated with Intercalating and Exfoliating a Sample

Compositions and methods associated with intercalating and exfoliating a sample are described herein. For example, of a method may include mixing the sample with intercalation materials. The intercalation materials are then intercalated into the sample to obtain a sample intercalated with the intercalation materials. The intercalated sample can then be exfoliated to produce an exfoliated sample.

Hung, Ching-Cheh↗

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 NTRS2018

Degradation of Intercalated Graphite Epoxy Composites Exposed to Low Earth Orbit

Four different graphite fiber/epoxy composites were exposed to the wake-side low Earth orbit (LEO) environment on the Optical Reflector Materials Experiment III (ORMatE-III) platform mounted on the exterior of the ISS for two years in order to determine their long term durability in the space environment. Three of the composite samples used bromine intercalated P100 fibers and one used pristine P100 fibers. One of the P100-Br samples was coated with a protective SiO2 layer, and half of another was coated with SiO2. Results were compared with the EOIM-III experiment which exposed the same materials in LEO in the ram direction for 42 h on the Space Shuttle. Although the atomic oxygen (AO) fluence of the ORMatE-III samples was one-third of the EOIM-III exposure, the resulting effects were qualitatively the same. Both found that SiO2 coated intercalated graphite composites showed no AO erosion, verifying that conventional protection strategies are applicable to bromine intercalated composites. Both found that bromine intercalation does not alter the AO erosion rates of graphite fiber/epoxy composites. Both found no bromine was detected to have migrated into the surrounding epoxy, even for highly eroded fibers and epoxy, allaying fears that bromination could compromise the properties of the epoxy. And both found no corrosive bromine was detected to have been released by the fibers allaying fears that outgassing could degrade sensitive electronics. The uncoated EOIM-III samples suffered slightly greater erosion resulting in a slightly higher solar absorptance. The general conclusion is that ram AO exposure had very similar effects on graphite fiber epoxy composites in both the EOIM-III and ORMatE-III experiments, and in neither case did bromine intercalation of the fibers substantially influence that degradation.

Intercalated graphite↗

NASA NTRS1971

Onset of superconductivity in sodium and potassium intercalated molybdenum disulphide

Molybdenum disulfide in the form of natural crystals or powder has been intercalated at -65 to -70 C with sodium and potassium using the liquid ammonia technique. All intercalated samples were found to show a superconducting transition. A plot of the percent of diamagnetic throw versus temperature indicates the possible existence of two phases in the potassium intercalated molybdenum disulfide. The onset of superconductivity in potassium and sodium intercalated molybdenite powder was found to be approximately 6.2 and approximately 4.5 K, respectively. The observed superconductivity is believed to be due to an increase in electron density as a result of intercalation.

Somoano, R. B.↗

NASA NTRS1972

Superconductivity in the alkali metal intercalates of molybdenum disulphide

The complete series of alkali metals, lithium through cesium, have been intercalated into molybdenum disulphide, using both the liquid ammonia and vapor techniques. All the intercalates with the exception of lithium yielded full superconducting transitions with onset temperatures of 6 K for AxMoS2(Ax=K,Rb,Cs) and 4 K for BxMoS2(Bx=Li,Na). The superconducting transition for lithium was incomplete down to 1.5 K. Stoichiometries and unit cell parameters have been determined for the intercalation compounds. Both rhombohedral and hexagonal polymorphs of MoS2 have been intercalated and found to exhibit the same superconductivity behavior. The nature of the extraneous superconducting transition of some intercalated samples on exposure to air was elucidated.

Somoano, R. B.↗

NASA NTRS1985

Homogeneity of pristine and bromine intercalated graphite fibers

Wide variations in the resistivity of intercalated graphite fibers and to use these materials for electrical applications, their bulk properties must be established. The homogeneity of the diameter, the resistivity, and the mass density of 50 graphite fibers, before and after bromine intercalation was measured. Upon intercalation the diameter was found to expand by about 5%, the resistivity to decrease by a factor of five, and the density to increase by about 6%. Each individual fiber was found to have uniform diameter and resistivity over macroscopic regions for lengths as long as 7 cm. The ratio of pristine to intercalated resistivity increases as the pristine fiber diameter increases at a rate of 0.16 micron, but decreases with the increasing ratio of intercalated diameter to pristine diameter at a rate of 0.08.

Gaier, J. R.↗

NASA NTRS1987

Stability of bromine, iodine monochloride, copper (II) chloride, and nickel (II) chloride intercalated pitch-based graphite fibers

Four different grades of pitch-based graphite fibers (Amoco P-55, P-75, P-100. and P-120) were intercalated with each of four different intercalates: bromine (Br2), iodine monochloride (ICl), copper (II) chloride (CuCl2), and nickel (II) chloride (NiCl2). The P-55 fibers did not react with Br2 or NiCl2, and the P-75 did not react with NiCl2. The stability of the electrical resistance of the intercalated fibers was monitored over long periods of time in ambient, high humidity (100 percent at 60 C), vacuum (10 to the -6 torr), and high temperature (up to 400 C) conditions. Fibers with lower graphitization form graphite intercalation compounds (GIC's) which are more stable than those with higher graphitization (i.e., P-55 (most stable) greater than P-75 greater than P-100 greater than P-120 (least stable). Br2 formed the most stable GIC's followed in order of decreasing stability by ICl, CuCl2, and NiCl2. While Br2 GIC's had the most stability, ICl had the advantages of forming GIC's with slightly greater reduction in resistance (by about 10%) than Br2, and the ability to intercalate P-55 fiber. Transition metal chlorides are susceptible to water vapor and high temperature. The stability of fibers in composites differs.

Gaier, James R.↗

NASA NTRS1988

Synthesis and stability of Br2, ICl and IBr intercalated pitch-based graphite fibers

The intercalation of halogens in pitch-based fiber is studied as well as the stability of the resultant intercalation compounds. It is found that IBr intercalates P-100 to yield a high-sigma GIC with attractive stability properties. During ICl intercalation, the presence of O2 interferes with the reaction and necessitates a higher threshold pressure for intercalation.

Wessbecher, Dorothy E.↗