Simultaneous electrical resistivity and mass uptake measurements in bromine intercalated fibers

Changes in mass and electrical resistivity of several types of pitch-based and vapor-grown graphite fibers were monitored during reaction with bromine. The observed threshold pressure dependent reaction suggested that the fibers were intercalated. In the fully brominated compound, the mass was increased by 44 percent and the resistivity was improved by a factor of 17. In the residue compound, the mass was increased by 22 percent and the resistivity was improved by a factor of 5. Fibers possessing different degrees of graphitization had surprisingly similar changes in both mass and resistivity

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

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

The effect of bromination of carbon fibers on the coefficient of thermal expansion of graphite fiber-epoxy composites

To examine the effect of bromination of carbon fibers on the coefficient of thermal expansion (CTE) of carbon fiber epoxy composites, several pristine and brominated carbon fiber-epoxy composite samples were subjected to thermomechanical analysis. The CTE's of these samples were measured in the uniaxial and transverse directions. The CTE was dominated by the fibers in the uniaxial direction, while it was dominated by the matrix in the transverse directions. Bromination had no effect on the CTE of any of the composites. In addition, the CTE of fiber tow was measured in the absence of a polymer matrix, using an extension probe. The results from this technique were inconclusive

Hot filament technique for measuring the thermal conductivity of molten lithium fluoride

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

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

Solar Selective Coatings Developed for Space Power Applications

A solar collector having the combined properties of high solar absorptance, low infrared emittance, and high thermal conductivity is envisioned for space power applications on minisatellites. A high solar absorptance is needed to collect as much of the incident solar radiation as possible and a low infrared emittance is needed to minimize radiant energy losses. A lightweight material having a high thermal conductivity is needed to transport the absorbed energy to where it is needed. Such a solar collector may be used with a low temperature-differential heat engine to provide electric power to the minisatellite components or as a source of thermal energy for a thermal bus that would heat remote regions of the spacecraft. The key to such a collector is the use of cermet coatings. Cermet coatings are composed of molecular islands of metal embedded in a three-dimensional matrix of dielectric. Recent research on molecular mixtures of aluminum and aluminum oxide at the NASA Glenn Research Center has yielded cermet coatings with a solar absorptance a of 0.797 and an infrared emittance epsilon of 0.131, yielding an alpha/epsilon ratio of 6. Although additional work is needed to further increase the alpha/epsilon ratio, these coatings are attractive owing to their potential durability in the space environment. The aluminum oxide surface should provide substantial protection from the atomic oxygen found in low Earth orbit. To help minimize emittance, these coatings are deposited on a smooth surface. The selected surface is aluminum that has been diamond turned to a mirror finish. Cermet coatings are manufactured by sputter deposition. To achieve the desired variable composition, Glenn's researchers implemented a novel approach using a cylindrical target composed of aluminum and aluminum oxide. Rotating the cylinder during the deposition process yields a coating of variable composition. A photograph of the custom-made aluminum and aluminum oxide cylindrical target installed in the sputter deposition chamber is shown

Determination of atomic oxygen fluence using spectrophotometric analysis of infrared transparent witness coupons for long duration exposure tests

Atomic oxygen degradation is one of several major threats to the durability of spaceborne systems in low Earth orbit. Ground-based simulations are conducted to learn how to minimize the adverse effects of atomic oxygen exposure. Assessing the fluence of atomic oxygen in test chambers such as a plasma asher over long periods of time is necessary for accurate determination of atomic oxygen exposure. Currently, an atomic oxygen susceptible organic material such as Kapton is placed next to samples as a witness coupon and its mass loss is monitored and used to determine the effective atomic oxygen fluence. However, degradation of the Kapton witness coupons occurs so rapidly in plasma ashers that for any long term test many witness coupons must be used sequentially in order to keep track of the fluence. This necessitates opening vacuum to substitute fresh coupons. A passive dosimetry technique was sought to monitor atomic oxygen exposure over longer periods without the need to open the plasma asher to the atmosphere. This paper investigates the use of spectrophotometric analysis of durable IR transparent witness coupons to measure atomic oxygen exposure for longer duration testing. The method considered would be conductive to making in situ measurements of atomic oxygen fluence

Correlation of Predicted and Observed Optical Properties of Multilayer Thermal Control Coatings

Thermal control coatings on spacecraft will be increasingly important, as spacecraft grow smaller and more compact. New thermal control coatings will be needed to meet the demanding requirements of next generation spacecraft. Computer programs are now available to design optical coatings and one such program was used to design several thermal control coatings consisting of alternating layers of WO3 and SiO2. The coatings were subsequently manufactured with electron beam evaporation and characterized with both optical and thermal techniques. Optical data were collected in both the visible region of the spectrum and the infrared. Predictions of solar absorptance and infrared emittance were successfully correlated to the observed thermal control properties. Functional performance of the coatings was verified in a bench top thermal vacuum chamber