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High temperature materials and graphite and composite program review to include: Baseline for unirradiated material properties, ASTM test development, design and construction rules (ASME-based), new fuel matrix mechanical studies, Irradiation damage studies, vender irradiation capsules, graphite supply chain worries, and ceramic composite activities.
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.
A commercial Czochralski crystal growing furnace was converted to a continuous growth facility by installation of a small, in-situ premelter with attendant silicon storage and transport mechanisms. Using a vertical, cylindrical graphite heater containing a small fused quartz test tube linear from which the molten silicon flowed out the bottom, approximately 83 cm of nominal 5 cm diamter crystal was grown with continuous melt addition furnished by the test tube premelter. High perfection crystal was not obtained, however, due primarily to particulate contamination of the melt. A major contributor to the particulate problem was severe silicon oxide buildup on the premelter which would ultimately drop into the primary melt. Elimination of this oxide buildup will require extensive study and experimentation and the ultimate success of continuous Czochralski depends on a successful solution to this problem. Economically, the continuous Czochralski meets near-term cost goals for silicon sheet material.
Procedures for quality control, fabrication techniques, specimen machining, test methodologies, and data collection and interpretation were defined using Thornel P-100 carbon fiber combined with Fiberite's 934 epoxy resin in unidirectional tape form. Tests on the prepreg material, including gel time, resin solids content, tack, volatile content, and flow are detailed. The steps of the fabrication and machining processes are described. Both destructive and nondestructive techniques were employed to assess the properties of the cured laminates. Tests to determine tensile strength and modulus, compressive strength and modulus, interlaminar and inplane shear strength, and flexural strength and modulus are discussed. The results of these experiments are compared with data generated by other researchers.
The flexural strength and average modulus of graphite fiber reinforced composites were tested before and after exposure to 0.5 Mev electron radiation and 1.33 Mev gamma radiation by using a three point bending test (ASTM D-790). The irradiation was conducted on vacuum treated samples. Graphite fiber/epoxy (T300/5208), graphite fiber/polyimide (C6000/PMR 15) and graphite fiber/polysulfone (C6000/P1700) composites after being irradiated with 0.5 Mev electron radiation in vacuum up to 5000 Mrad, show increases in stress and modulus of approximately 12% compared with the controls. Graphite fiber/epoxy (T300/5208 and AS/3501-6), after being irradiated with 1.33 Mev gamma radiation up to 360 Mrads, show increases in stress and modulus of approximately 6% at 167 Mrad compared with the controls. Results suggest that the graphite fiber composites studied should withstand the high energy radiation in a space environment for a considerable time, e.g., over 30 years.
The feasibility of applying the in situ fiberization process to the fabrication of strain isolation pads (SIP) for the Space Shuttle and to the fabrication of graphite-epoxy composites was evaluated. The ISF process involves the formation of interconnected polymer fiber networks by agitation of dilute polymer solutions under controlled conditions. High temperature polymers suitable for SIP use were fiberized and a successful fiberization of polychloro trifluoroethylene, a relatively high melting polymer, was achieved. Attempts to fiberize polymers with greater thermal stability were unsuccessful, apparently due to characteristics caused by the presence of aromaticity in the backbone of such materials. Graphite-epoxy composites were fabricated by interconnecting two dimensional arrays of graphite fiber with polypropylene IS fibers with subsequent epoxy resin impregnation. Mechanical property tests were performed on laminated panels of this material to evaluate intralaminar and interlaminar shear strength, and thus fracture toughness. Test results were generally unpromising.
Eight-ply quasi-isotropic composite plates of Thornel 300 graphite in Narmco 5208 epoxy resin (T300/5208) were tested to establish the degree of equivalence between low-velocity impact and static testing. Both the deformation and failure mechanics under impact were representable by static indentation tests. Under low-velocity impacts such as tool drops, the dominant deformation mode of the plates was the first, or static, mode. Higher modes are excited on contact, but they decay significantly by the time the first-mode load reaches a maximum. The delamination patterns were observed by X-ray analysis. The areas of maximum delamination patterns were observed by X-ray analysis. The areas of maximum delamination coincided with the areas of highest peel stresses. The extent of delamination was similar for static and impact tests. Fiber failure damage was established by tensile tests on small fiber bundles obtained by deplying test specimens. The onset of fiber damage was in internal plies near the lower surface of the plates. The distribution and amount of fiber damage was similar fo impact and static tests.
A full scale section of a transport aircraft wing box was designed, analyzed, fabricated, and tested. The wing box section, which was called the technology integration box beam, contained blade stiffened covers and T-stiffened channel spars constructed using graphite-epoxy materials. Covers, spars, and the aluminum ribs were assembled using mechanical fasteners. The box beam was statically tested for several loading conditions to verify the stiffness and strength characteristics of the composite wing design. Failure of the box beam occurred at 125 pct. of design limit load during the combined unbending and torsion ultimate design load test. It appears that the failure initiated at a stiffener runout location in the upper cover which resulted in rupture of the upper cover and portions of both spars.
This interim report documents preliminary results of the post-irradiation examination material property testing from the fourth advanced graphite creep (AGC), AGC 4, capsule specimens. This is the fourth of a series of six irradiation test trains planned as part of the AGC experiment to fully characterize the neutron irradiation effects and radiation creep behavior of current nuclear graphite grades to moderate dose levels (=7 dpa). The AGC 4 capsule was irradiated in the Idaho National Laboratory Advanced Test Reactor at a nominal temperature of 800°C and to a peak dose of 8 dpa. Half of the AGC-4 specimens were subjected to compressive stresses to induce irradiation creep. Post-irradiation testing and measurement results are reported with the exception of thermal testing, which is still in progress, and irradiation mechanical strength testing. Additionally, some specimens initially deemed too hot to be examined in the ART Graphite laboratory may still be measured. The data reported includes specimen dimensions for both stressed and unstressed specimens to establish the irradiation creep rates, mass and dimensional data necessary to derive density, elastic constants (Young?s modulus, shear modulus, and Poisson?s ratio) from ultrasonic time of flight velocity measurements, Young?s modulus from the fundamental frequency of vibration, and electrical resistivity. A more complete evaluation of trends in the material property changes, as well as irradiation-induced creep due to the irradiation environment and applied load on the specimens, will be discussed later in AGC 4 post-irradiation examination analysis reports.
This interim report documents preliminary results of the post-irradiation examination material property testing from the fourth advanced graphite creep (AGC), AGC 4, capsule specimens. This is the fourth of a series of six irradiation test trains planned as part of the AGC experiment to fully characterize the neutron irradiation effects and radiation creep behavior of current nuclear graphite grades to moderate dose levels (=7 dpa). The AGC 4 capsule was irradiated in the Idaho National Laboratory Advanced Test Reactor at a nominal temperature of 800°C and to a peak dose of 8 dpa. Half of the AGC-4 specimens were subjected to compressive stresses to induce irradiation creep. Post-irradiation testing and measurement results are reported with the exception of thermal testing, which is still in progress, and irradiation mechanical strength testing. Additionally, some specimens initially deemed too hot to be examined in the ART Graphite laboratory may still be measured. The data reported includes specimen dimensions for both stressed and unstressed specimens to establish the irradiation creep rates, mass and dimensional data necessary to derive density, elastic constants (Young?s modulus, shear modulus, and Poisson?s ratio) from ultrasonic time of flight velocity measurements, Young?s modulus from the fundamental frequency of vibration, and electrical resistivity. A more complete evaluation of trends in the material property changes, as well as irradiation-induced creep due to the irradiation environment and applied load on the specimens, will be discussed later in AGC 4 post-irradiation examination analysis reports.
The paper considers different material concepts that can be fabricated of hybridized composites which demonstrate improved graphite fiber retention capability in a severe fire without significant reduction to the composite properties. More than 30 panels were fabricated for mechanical and fire tests, the details and results of which are presented. Methods of composite hybridization investigated included the addition of oxidation resistant fillers to the resin, mechanically interlocking the graphite fibers by the use of woven fabrics, and the addition of glass fibers and glass additives designed to melt and fuse the graphite fibers together. It is concluded that a woven fabric with a serving of glass around each graphite tow is by far the superior of those evaluated: not only is there a coalescing effect in each graphite layer, but there is also a definite adhesion of each layer to its neighbor.
A mathematical model predicting the strength of unidirectional fiber reinforced composites containing known flaws and with linear elastic-brittle material behavior was developed. The approach was to imbed a local heterogeneous region surrounding the crack tip into an anisotropic elastic continuum. This (1) permits an explicit analysis of the micromechanical processes involved in the fracture, and (2) remains simple enough to be useful in practical computations. Computations for arbitrary flaw size and orientation under arbitrary applied loads were performed. The mechanical properties were those of graphite epoxy. With the rupture properties arbitrarily varied to test the capabilities of the model to reflect real fracture modes, it was shown that fiber breakage, matrix crazing, crack bridging, matrix-fiber debonding, and axial splitting can all occur during a period of (gradually) increasing load prior to catastrophic failure. The calculations also reveal the sequential nature of the stable crack growth process proceding fracture.
A mathematical model for the strength of fiber reinforced composites containing specific flaws is described. The approach is to embed a local heterogeneous region surrounding the crack tip in an anisotropic elastic continuum. By consideration of the individual failure events activated near the flaw tip, a strength prediction can be made from basic properties of the composite constituents. Computations for arbitrary flaw size and orientation have been performed for unidirectional composites with linear elastic-brittle constituent behavior. The mechanical properties were those of graphite epoxy. With the rupture properties arbitrarily varied to test the capability of the model to reflect real fracture modes in fiber composites, it is shown that fiber breakage, matrix crazing, crack bridging, matrix-fiber debonding, and axial splitting all can occur during gradually increasing load prior to catastrophic fracture. Qualitative comparisons with experimental results on edge-notched unidirectional graphite epoxy specimens have also been made.
A broad group of fibers and matrices were combined to create a wide range of composite properties. Primary material fabrication procedures were developed which readily permit the fabrication of flat plate and shaped composites. Composite mechanical properties were measured under a wide range of test conditions. Tensile, flexure mechanical fatigue, thermal fatigue, fracture toughness, and fatigue crack growth resistance were evaluated. Selected fiber-matrix combinations were shown to maintain their strength at up to 1300 K when tested in an inert atmosphere. Composite high temperature mechanical properties were shown to be limited primarily by the oxidation resistance of the graphite fibers. Composite thermal dimensional stability was measured and found to be excellent.
The application of the Iosipescu shear test for the room and high temperature failure analyses of the woven graphite/polyimide composites with the medium (T-650) and igh (M40J and M60J) modulus graphite fibers is discussed. The M40J/PMR-II-50 and M60J/PMR-II-50 composites were tested as supplied and after thermal conditioning. The effect of temperature and conditioning on the initiation of intralaminar damage and the shear strength of the composites was established.
A mathematical model is described which will permit predictions of the strength of fiber reinforced composites containing known flaws to be made from the basic properties of their constituents. The approach was to embed a local heterogeneous region (LHR) surrounding the crack tip into an anisotropic elastic continuum. The model should (1) permit an explicit analysis of the micromechanical processes involved in the fracture process, and (2) remain simple enough to be useful in practical computations. Computations for arbitrary flaw size and orientation under arbitrary applied load combinations were performed from unidirectional composites with linear elastic-brittle constituent behavior. The mechanical properties were nominally those of graphite epoxy. With the rupture properties arbitrarily varied to test the capability of the model to reflect real fracture modes in fiber composites, it was shown that fiber breakage, matrix crazing, crack bridging, matrix-fiber debonding, and axial splitting can all occur during a period of (gradually) increasing load prior to catastrophic fracture. The computations reveal qualitatively the sequential nature of the stable crack process that precedes fracture.
The results of an experimental program are described which establishes the feasibility and guide lines for resin development. The objective was to identify the basic epoxy neat resin properties that improve low velocity impact resistance and toughness to graphite-epoxy laminates and at the same time maintain useful structural laminate mechanical properties. Materials tests from twenty-three toughened epoxy resin matrix systems are included.
Design approaches and materials are described from which are fabricated pyrostatic graphite/epoxy (Gr/Ep) laminates that show improved retention of graphite particulates when subjected to burning. Sixteen hybridized plus two standard Gr/Ep laminates were designed, fabricated, and tested in an effort to eliminate the release of carbon (graphite) fiber particles from burned/burning, mechanically disturbed samples. The term pyrostatic is defined as meaning mechanically intact in the presence of fire. Graphite particulate retentive laminates were constructed whose constituent materials, cost of fabrication, and physical and mechanical properties were not significantly different from existing Gr/Ep composites. All but one laminate (a Celion graphite/bis-maleimide polyimide) were based on an off-the-shelf Gr/Ep, the AS-1/3501-5A system. Of the 16 candidates studied, four thin (10-ply) and four thick (50-ply) hybridized composites are recommended.