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Article discusses procedure where hydrazine is used to extract graphite fibers from cured polyimide resin. Method does not attack graphite fibers and is faster than hot-concentrated-acid digestion process.
An action plan formulated to address the rapid growth in the use of graphite reinforced composite materials and the potential for the release of free fibers is outlined. The role of various agencies with respect to the civil sector of the user community is discussed. Emphasis is placed on NASA responsibilities in the area of quantifying the risk associated with the use of graphite bearing composites in aircraft.
Activities described include: (1) determining the applicability of an ultrahigh-strength graphite fiber to composite pressure vessels; (2) defining the fatigue performance of thin-titanium-lined, high-strength graphite/epoxy pressure vessel; (3) selecting epoxy resin systems suitable for filament winding; (4) studying the fatigue life potential of Kevlar 49/epoxy pressure vessels; and (5) developing polymer liners for composite pressure vessels. Kevlar 49/epoxy and graphite fiber/epoxy pressure vessels, 10.2 cm in diameter, some with aluminum liners and some with alternation layers of rubber and polymer were fabricated. To determine liner performance, vessels were subjected to gas permeation tests, fatigue cycling, and burst tests, measuring composite performance, fatigue life, and leak rates. Both the metal and the rubber/polymer liner performed well. Proportionately larger pressure vessels (20.3 and 38 cm in diameter) were made and subjected to the same tests. In these larger vessels, line leakage problems with both liners developed the causes of the leaks were identified and some solutions to such liner problems are recommended.
Flexture and short beam shear specimens of a graphite epoxy and a graphite polymimide composite material were tested in an arc tunnel environment. The materials were subjected to seven heating rates from 12.5 to 308 kW/sw m for test times from 5 to 1000 seconds. The temperature response of the specimens was measured and the strength degradation caused by the various heating environments was determined.
Flexible solar-array substrates, graphite-fiber/epoxy - aluminum honeycomb panels, and thin dielectric films were exposed to monoenergetic electron beams ranging in energy from 2 to 20 keV in the Lewis Research Center's geomagnetic-substorm-environment simulation facility to determine surface potentials, dc currents, and surface discharges. The four solar-array substrate samples consisted of Kapton sheet reinforced with fabrics of woven glass or carbon fibers. They represented different construction techniques that might be used to reduce the charge accumulation on the array back surface. Five honeycomb-panel samples were tested, two of which were representative of Voyager antenna materials and had either conductive or nonconductive painted surfaces. A third sample was of Navstar solar-array substrate material. The other two samples were of materials proposed for use on Intelsat V. All the honeycomb-panel samples had graphite-fiber/epoxy composite face sheets. The thin dielectric films were 2.54-micrometer-thick Mylar and 7.62-micrometer-thick Kapton.
The potential of cyanate resins as replacement for epoxy resins in composites with graphite fiber reinforcement was investigated in an effort to provide improved moisture resistance and toughness in laminating systems at a projected cost, handleability, and processing requirements equivalent to 400 K (260 F) curing epoxies. Monomer synthesis, formulation, blending, resin preparation, catalysis studies, prepreg preparation, laminate fabrication, and testing are discussed. A graphite fiber reinforced laminate was developed with 95 percent retention of the original 363 K (180 F) flexural strength and 70 percent retention of the 363 K (180 F) short beam shear strength after 500 hour exposure to 95 + 7 relative humidity at 324 K (120 F).
The development of a vacuum die-casting process for producing silicon sheet suitable for photovoltaic cells with a terrestrial efficiency greater than 12 percent and having the potential to be scaled for large quantity production is considered. The initial approach includes: (1) obtaining mechanical design parameters by using boron nitride, which has been shown to non-wetting to silicon; (2) optimizing silicon nitride material composition and coatings by sessile drop experiments; (3) testing effectiveness of fluoride salt interfacial media with a graphite mold; and (4) testing the effect of surface finish using both boron nitride and graphite. When the material and mechanical boundary conditions are established, a finalized version of the prototype assembly will be constructed and the casting variables determined.
Composite materials are discussed with reference to their mechanical and physical properties, fatigue and fracture testing and analysis, nondestructive evaluation, fabrication, and commercial applications. Particular papers are presented on such topics as analysis of mechanical strength data from hybrid laminates of glass and graphite fibers, graphite-aluminum composites, the mechanical behavior of molybdenum-reinforced metal composites, and composite laminate application in magnetic fusion energy superconducting magnet systems.
The development of composites in the United States in the 1960s and 1970s is briefly reviewed with emphasis on aerospace applications. Consideration is given to such highlights as the manufacture of boron filaments, the use of boron-epoxy composites for aerospace structures, graphite-epoxy composites, and current graphite R & D work.
Hard wear-resistant coatings and soft low shear strength coatings were developed for an air-lubricated compliant journal bearing for a future automotive gas turbine engine. The coatings were expected to function in either 540 or 650 C ambient. Soft lubricant coatings were generally limited in temperature. Therefore emphasis was on the hard wear-resistant coatings. The coating materials covered were TiC, B4C, Cr3C2, WC, SiC, CrB2, TiB2, Cr2O3, Al2O3, Si3N4, Tribaloy 800, CaF2, CaF2-BaF2 eutectic, Ni-Co, silver, CdO-graphite and proprietary compounds. The coatings on test coupons were subjected to static oven screening tests. The test consisted of exposure of material samples in an oven for 300 h at the maximum temperature (540 or 650 C) and ten temperature cycles from room temperature to the maximum service temperature. On the basis of the specimen examinations the following coatings were recommended for future wear tests: TiC (sputtered), Cr2O3 (sputtered), Si3N4 (sputtered), CdO and graphite (fused), Kaman DES (a proprietary coating), CrB2 (plasma sprayed), Cr3C2 (detonation gun) and NASA PS-106 (plasma sprayed).
This paper describes the test program of a lightweight 25 kW solar array for solar electric propulsion. A full-scale development wing was made of aluminum with the containment box cover of graphite-epoxy, while the flight design array wing uses a graphite-epoxy structure. The full-scale continuous longeron array extension mast was tested for performance on a water table, and the full scale wing was functionally tested to demonstrate automatic containment box unlocking, wing extension, and retraction, blanket tensioning, and automatic application of blanket preload. The wing was then tested to the Shuttle acoustic environment, followed by a thermal/vacuum test in which the wing was extended and retracted at high and low temperature. Finally, the wing was tested in vibration with sine and random vibration environments.
A second generation polymerization monomeric reactants (PMR) polyimdes matrix system (PMR 2) was characterized in both neat resin and composite form with two different graphite fiber reinforcements. Three different formulated molecular weight levels of laboratory prepared PMR 2 were examined, in addition to a purchased experimental fully formulated PMR 2 precurser solution. Isothermal aging of graphite fibers, neat resin samples and composite specimens in air at 316 C were investigated. Humidity exposures at 65 C and 97 percent relative humidity were conducted for both neat resin and composites for eight day periods. Anaerobic char of neat resin and fire testing of composites were conducted with PMR 15, PMR 2, and an epoxy system. Composites were fire tested on a burner rig developed for this program. Results indicate that neat PMR 2 resins exhibit excellent isothermal resistance and that PMR 2 composite properties appear to be influenced by the thermo-oxidative stability of the reinforcing fiber.
Graphite fiber reinforced resin matrix composites were subjected to controlled burning conditions to determine their burning characteristics and fiber retention properties. Small samples were burned with a natural gas fired torch to study the effects of fiber orientation and structural flaws such as holes and slits that were machined into the laminates. Larger laminate samples were burned in a modified heat release rate calorimeter. Unidirectional epoxy/graphite and polyimide/graphite composites and boron powder filled samples of each of the two composite systems were burn tested. The composites were exposed to a thermal radiation of 5.3 Btu/sq ft-sec in air. Samples of each of the unfilled composite were decomposed anaerobically in the calorimeter. Weight loss data were recorded for burning and decomposition times up to thirty-five minutes. The effects of fiber orientation, flaws, and boron filler additives to the resins were evaluated. A high char forming polyimide resin was no more effective in retaining graphite fibers than a low char forming epoxy resin when burned in air. Boron powder additions to both the polyimide and the epoxy resins stabilized the chars and effectively controlled the fiber release.
The design and analysis of a composite fan blade for the under the wing (UTW) QCSEE is presented. The blade is designed for a variable pitch, 18 bladed rotor and is constructed from a hybrid composite combination of materials consisting of Kevlar-49, type AS graphite, boron, and S-glass fibers in a PR288 epoxy resin matrix. The blade has an attached platform which is constructed of AS-graphite, PR288 epoxy resin matrix and aluminum honeycomb. The blade is designed to satisfy aerostability and cyclic life and strength requirements with a light weight construction. The attached platform is designed for a fail-safe condition in that it is retainable by the blade, under centrifugal force loading, even in the event of blade to platform bond separation. Details of the blade design and the results of stress, vibration, and impact analysis are included.
A suitable method for the direct measurement of moisture concentrations after humidity/thermal exposure on state of the art epoxy and polyimide resins and their graphite and glass fiber reinforcements was investigated. Methods for the determination of moisture concentration profiles, moisture diffusion modeling and moisture induced chemical changes were examined. Carefully fabricated, precharacterized epoxy and polyimide neat resins and their AS graphite and S glass reinforced composites were exposed to humid conditions using heavy water (D20), at ambient and elevated temperatures. These specimens were fixtured to theoretically limit the D20 permeation to a unidirectional penetration axis. The analytical techniques evaluated were: (1) laser pyrolysis gas chromatography mass spectrometry; (2) solids probe mass spectrometry; (3) laser pyrolysis conventional infrared spectroscopy; and (4) infrared imaging thermovision. The most reproducible and sensitive technique was solids probe mass spectrometry. The fabricated exposed specimens were analyzed for D20 profiling after humidity/thermal conditioning at three exposure time durations.
Basic manufacturing method refinements for using graphite epoxy material for a nickel cadmium battery cell case were performed to demonstrate production feasibility. The various facets of production scale-up, i.e., process and tooling development, together with material and process control, were integrated into a comprehensive manufacturing process that assures production reproducibility and product uniformity. Test results substantiate that a battery cell case produced from graphite epoxy pre-impregnated material, utilizing the internal pressure bag fabrication method, is feasible.
Carbon/graphite fibers were chemically oxidized in the liquid phase to fibers of graphite oxide. Resistivity increases as high as 10,000 times were obtained, the oxidized fiber decomposed on exposure to atmosphere. A factor of 1,000 remained as a stable increment. The largest change observed was 1,000,000 times. Best results were obtained on the most highly graphitized fibers. Electrochemical oxidation yielded a lower increase--about 10 times, but provided a controllable method of synthesis and insight to the mechanism of reaction. Tensile tests indicated that the strength of the fiber on oxidation was decreased by no more than 25 percent.
Avionics components commonly used in commercial aircraft were tested for vulnerability to failure when operated in an environment with a high density of graphite fibers. The components were subjected to a series of exposures to graphite fibers of different lengths. Lengths used for the tests were (in order) 1 mm, 3 mm, and 10 mm. The test procedure included subjecting the equipment to characteristic noise and shock environments. Most of the equipment was invulnerable or did not fail until extremely high average exposures were reached. The single exception was an air traffic control transponder produced in the early 1960's. It had the largest case open area through which fibers could enter and it had no coated boards.