Current research in oxidation-resistant carbon-carbon composites at NASA. Langley Research Center

The significant potential of carbon-carbon composites for high-temperature structural applications is well established. For hypersonic vehicle applications, desirable properties include low density, high specific strength and stiffness, low coefficients of thermal expansion, and retention of mechanical properties above 3000 F. A significant problem associated with carbon materials, however, is that they oxidize rapidly in air at temperatures above about 800 F, and therefore must be protected from oxidation. Successful development of effective methods of oxidation protection is key to the eventual utilization of carbon-carbon composites on hypersonic vehicles such as NASP. In this presentation, the basic elements of an oxidation-protection system are described. Results from oxidation-performance evaluations of state-of-the-art ACC-4 type material in simulated airframe vehicle environments (temperature, pressure, and time) conducted at NASA Langley are also presented. NASA Langley has an active research effort to improve the oxidation resistance of carbon-carbon materials for airframe structural and vehicle thermal protection applications. Conversion coating and sealant development research is highlighted

NASA Langley Research Center National Aero-Space Plane Mission simulation profile sets

To provide information on the potential for long life service of oxidation resistant carbon-carbon (ORCC) materials in the National Aero-Space Plane (NASP) airframe environment, NASP ascent, entry, and cruise trajectories were analytically flown. Temperature and pressure profiles were generated for 20 vehicle locations. Orbital (ascent and entry) and cruise profile sets from four locations are presented along with the humidity exposure and testing sequences that are being used to evaluate ORCC materials. The four profiles show peak temperatures during the ascent leg of an orbital mission of 2800, 2500, 2000, and 1700 F. These profiles bracket conditions where carbon-carbon might be used on the NASP vehicle

Compression Testing of Alumina Fiber Insulation

A series of tests were conducted to measure the response of alumina fiber insulation to compression loading. The alumina fiber insulation is a candidate gasket material for the Space Shuttle Government Furnished Equipment (GFE) Tile Overlay Repair. Tests were conducted at room temperature and 2300 F. The alumina fiber insulation is a fibrous insulation blanket which was supplied to Langley in two forms, a nominal 3 lb/ft3 version and a nominal 9 lb/ft3 version. The 3 lb/ft3 material was tested as sheets 0.15 and 0.25 inches thick and the 9 lb/ft3 material in sheets 1 inch thick. The material showed very non-linear compression behavior with the compressive resistance of the material increasing as the material was compressed. The 3 lb/ft3 0.15-inch thick material required 4.1 psi to reach the nominal installation thickness of 0.045 inches and retain a load of 2.1 lbs during unloading. Testing at 2300 F resulted in a stiffer more board-like material. The 3 lb/ft3 0.15-inch thick material retained 1 psi of compressive resistance after a 10 minute hold at 2300 F and 0.045 inches thickness

Effect of Test Specimen Shape and Size on Interlaminar Tensile Properties of Advanced Carbon-Carbon Composites

The interlaminar tensile strength of 1000-tow T-300 fiber ACC-6 carbon-carbon composites was measured using the method of bonding the coupons to adherends at room temperature. The size, 0.70 to 1.963 inches maximum width or radius, and shape, round or square, of the test coupons were varied to determine if the test method was sensitive to these variables. Sixteen total variations were investigated and the results modeled

Four advances in carbon-carbon materials technology

Carbon-carbon composites are a specialty class of materials having many unique properties making these composites attractive for a variety of demanding engineering applications. Chief among these properties are exceptional retention of mechanical properties at temperatures as high as 4000 F, excellent creep resistance, and low density (1.6 to 1.8 g/cu cm). Although carbon-carbon composites are currently in service in a variety of applications, much development work remains to be accomplished before these materials can be considered to be fully mature, realizing their full potential. Four recent technology advances holding particular promise for overcoming current barriers to the wide-spread commercialization of carbon-carbon composites are described. These advances are: markedly improved interlaminar strengths (more than doubled) of two dimensional composites achieved by whiskerization of the fabric reinforcing plies, simultaneously improved oxidation resistance and mechanical properties achieved by the incorporation of matrix-phase oxidation inhibitors based on carborane chemistry, improved oxidation resistance achieved by compositionally graded oxidation protective coatings, and markedly reduced processing times (hours as opposed to weeks or months) accomplished through a novel process of carbon infiltration and coatings deposition based on the use of liquid-phase precursor materials

Creep Forming of Carbon-Reinforced Ceramic-Matrix Composites

A set of lecture slides describes an investigation of creep forming as a means of imparting desired curvatures to initially flat stock plates of carbon-reinforced ceramic-matrix composite (C-CMC) materials. The investigation is apparently part of a continuing effort to develop improved means of applying small CCMC repair patches to reinforced carbon-carbon leading edges of aerospace vehicles (e.g., space shuttles) prior to re-entry into the atmosphere of the Earth. According to one of the slides, creep forming would be an intermediate step in a process that would yield a fully densified, finished C-CMC part having a desired size and shape (the other steps would include preliminary machining, finish machining, densification by chemical vapor infiltration, and final coating). The investigation included experiments in which C-CMC disks were creep-formed by heating them to unspecified high temperatures for time intervals of the order of 1 hour while they were clamped into single- and double-curvature graphite molds. The creep-formed disks were coated with an oxidation- protection material, then subjected to arc-jet tests, in which the disks exhibited no deterioration after exposure to high-temperature test conditions lasting 490 seconds

Improved Test Planning and Analysis Through the Use of Advanced Statistical Methods

The goal of this work is, through computational simulations, to provide statistically-based evidence to convince the testing community that a distributed testing approach is superior to a clustered testing approach for most situations. For clustered testing, numerous, repeated test points are acquired at a limited number of test conditions. For distributed testing, only one or a few test points are requested at many different conditions. The statistical techniques of Analysis of Variance (ANOVA), Design of Experiments (DOE) and Response Surface Methods (RSM) are applied to enable distributed test planning, data analysis and test augmentation. The D-Optimal class of DOE is used to plan an optimally efficient single- and multi-factor test. The resulting simulated test data are analyzed via ANOVA and a parametric model is constructed using RSM. Finally, ANOVA can be used to plan a second round of testing to augment the existing data set with new data points. The use of these techniques is demonstrated through several illustrative examples. To date, many thousands of comparisons have been performed and the results strongly support the conclusion that the distributed testing approach outperforms the clustered testing approach

Emissivity Results on High Temperature Coatings for Refractory Composite Materials

The directional emissivity of various refractory composite materials considered for application for reentry and hypersonic vehicles was investigated. The directional emissivity was measured at elevated temperatures of up to 3400 F using a directional spectral radiometric technique during arc-jet test runs. A laboratory-based relative total radiance method was also used to measure total normal emissivity of some of the refractory composite materials. The data from the two techniques are compared. The paper will also compare the historical database of Reinforced Carbon-Carbon emissivity measurements with emissivity values generated recently on the material using the two techniques described in the paper

Development of X-43A Mach 10 Leading Edges

The nose leading edge of the Hyper-X Mach 10 vehicle was orginally anticipated to reach temperatures near 4000 F at the leading-edge stagnation line. A SiC coated carbon/carbon (C/C) leading-edge material will not survive that extreme temperature for even a short duration single flight. To identify a suitable leading edge for the Mach 10 vehicle, arc-jet testing was performed on thirteen leading-edge segments fabricated from different material systems to evaluate their performance in a simulated flight environment. Hf, Zr, Si, and Ir based materials, in most cases as a coating on C/C, were included in the evaluation. Afterwards, MER, Tucson, AZ was selected as the supplier of the flight vehicle leading edges. The nose and the vertical and horizontal tail leading edges were fabricated out of a 3:1 biased high thermal conductivity C/C. The leading edges were coated with a three layer coating comprised of a SiC conversion of the top surface of the C/C, followed by a chemical vapor deposited layer of SiC, followed by a thin chemical vapor deposited layer of HfC. This paper will describe the fabrication of the Mach 10 C/C leading edges and the testing performed to validate performance

Lethal Antibody Enhancement of Dengue Disease in Mice Is Prevented by Fc Modification

Immunity to one of the four dengue virus (DV) serotypes can increase disease severity in humans upon subsequent infection with another DV serotype. Serotype cross-reactive antibodies facilitate DV infection of myeloid cells in vitro by promoting virus entry via Fcγ receptors (FcγR), a process known as antibody-dependent enhancement (ADE). However, despite decades of investigation, no in vivo model for antibody enhancement of dengue disease severity has been described. Analogous to human infants who receive anti-DV antibodies by transplacental transfer and develop severe dengue disease during primary infection, we show here that passive administration of anti-DV antibodies is sufficient to enhance DV infection and disease in mice using both mouse-adapted and clinical DV isolates. Antibody-enhanced lethal disease featured many of the hallmarks of severe dengue disease in humans, including thrombocytopenia, vascular leakage, elevated serum cytokine levels, and increased systemic viral burden in serum and tissue phagocytes. Passive transfer of a high dose of serotype-specific antibodies eliminated viremia, but lower doses of these antibodies or cross-reactive polyclonal or monoclonal antibodies all enhanced disease in vivo even when antibody levels were neutralizing in vitro. In contrast, a genetically engineered antibody variant (E60-N297Q) that cannot bind FcγR exhibited prophylactic and therapeutic efficacy against ADE-induced lethal challenge. These observations provide insight into the pathogenesis of antibody-enhanced dengue disease and identify a novel strategy for the design of therapeutic antibodies against dengue