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NASA NTRS2003

Ultra-High-Temperature Ceramics Evaluated for Aeropropulsion Use

Ultra-high-temperature ceramics (UHTC) are a group of materials consisting of zirconium diboride (ZrB2) or hafnium diboride (HfB2) plus silicon carbide (SiC), and in some instances, carbon (C). They offer a combination of properties that make them candidates for airframe leading edges on sharp-bodied reentry vehicles. These UHTCs perform well in the environment for such applications (i.e., air at low pressures). The purpose of this study at the NASA Glenn Research Center was to examine three of these materials under conditions more representative of a propulsion environment: that is, higher oxygen partial pressure and total pressure. Relatively long, multiple-exposure cycles were emphasized. We completed an in-house study of ZrB2 plus 20 vol% SiC (abbreviated as ZS), ZrB2 plus 14 vol% SiC and 30 vol% C (ZSC), and SCS-9a SiC fiber-reinforced ZrB2 plus 20 vol% SiC (ZSS). HfB2-based compositions were not included in the study because of their high cost. The capability of UHTC for propulsion applications must be compared with that of mature, available, and commercially used ceramics such as silicon nitride (e.g., AS-800) to put things in proper perspective. In terms of mechanical properties, UHTCs fall short in terms of strength and fracture toughness. At about 1300 C, the creep resistance of ZS appears to be superior to the creep resistance reported for AS-800. However, the stress rupture life for Si3N4 under stress and temperature conditions similar to those used in this study is measured in hundreds of hours. Because of oxidation, ZS could not achieve such lives. In terms of oxidation resistance, acceptable amounts of material recession in 1 hour to thousands of hours, depending on the specific propulsion application, are on the order of 100 to 300 mm. This converts to an acceptable range of parabolic recession rate constants kp" of approximately less than or equal to 10(exp -1) to 10(exp -2) square millimeters per hour for a 1-hr application. For a 100-hr application, an acceptable range of kp" would be less than or equal to those values divided by 100. For the more oxidation resistant ZS material, measured parabolic recession rate constants were 4.7 x 10(exp -3) millimeters per hour at 1327 C, 7.8 x 10(exp -2) square millimeters per hour at 1627 C, and 1.3 millimeters per hour at 1927 C. Thus, recession rate constants for ZS are acceptable at 1327 C for a 1-hr application, but here silicon nitride is a superior material. At 1627 C, ZS oxidation is marginal for a 1-hr application, but dimensional growth would be an issue. In a 100-hr application, ZS cannot be considered at any temperature. Our cursory examination of thermal shock, both from a theoretical and experimental viewpoint, indicated that the ZS and ZSC UHTCs are inferior to AS-800 silicon nitride. On the basis of this limited study, UHTCs are not ready to be considered as aeropropulsion materials for any applications longer than a few minutes. Current materials suffer from aggressive oxidation and moisture attack (Quynhgiao Nguyen, NASA Glenn, and Raymond C. Robinson, QSS Group, Inc., Cleveland, OH, 2002, private communication), and they are susceptible to thermal shock. For long-term propulsion applications, major improvements in environmental durability are needed. Work is in progress to improve the oxidation resistance of UHTC materials.

Levine, Stanley R.↗

NASA NTRS2003

Structural Anomalies Detected in Ceramic Matrix Composites Using Combined Nondestructive Evaluation and Finite Element Analysis (NDE and FEA)

Most reverse engineering approaches involve imaging or digitizing an object and then creating a computerized reconstruction that can be integrated, in three dimensions, into a particular design environment. The rapid prototyping technique builds high-quality physical prototypes directly from computer-aided design files. This fundamental technique for interpreting and interacting with large data sets is being used here via Velocity2 (an integrated image-processing software, ref. 1) using computed tomography (CT) data to produce a prototype three-dimensional test specimen model for analyses. A study at the NASA Glenn Research Center proposes to use these capabilities to conduct a combined nondestructive evaluation (NDE) and finite element analysis (FEA) to screen pretest and posttest structural anomalies in structural components. A tensile specimen made of silicon nitrite (Si3N4) ceramic matrix composite was considered to evaluate structural durability and deformity. Ceramic matrix composites are being sought as candidate materials to replace nickel-base superalloys for turbine engine applications. They have the unique characteristics of being able to withstand higher operating temperatures and harsh combustion environments. In addition, their low densities relative to metals help reduce component mass (ref. 2). Detailed three-dimensional volume rendering of the tensile test specimen was successfully carried out with Velocity2 (ref. 1) using two-dimensional images that were generated via computed tomography. Subsequent, three-dimensional finite element analyses were performed, and the results obtained were compared with those predicted by NDE-based calculations and experimental tests. It was shown that Velocity2 software can be used to render a three-dimensional object from a series of CT scan images with a minimum level of complexity. The analytical results (ref. 3) show that the high-stress regions correlated well with the damage sites identified by the CT scans and the experimental data. Furthermore, modeling of the voids collected via NDE offered an analytical advantage that resulted in more accurate assessments of the material s structural strength. The top figure shows a CT scan image of the specimen test section illustrating various hidden structural entities in the material and an optical image of the test specimen considered in this study. The bottom figure represents the stress response predicted from the finite element analyses (ref .3 ) for a selected CT slice where it clearly illustrates the correspondence of the high stress risers due to voids in the material with those predicted by the NDE. This study is continuing, and efforts are concentrated on improving the modeling capabilities to imitate the structural anomalies as detected.

Abdul-Aziz, Ali↗

NASA NTRS2004

Integrity of Ceramic Parts Predicted When Loads and Temperatures Fluctuate Over Time

Brittle materials are being used, and being considered for use, for a wide variety of high performance applications that operate in harsh environments, including static and rotating turbine parts for unmanned aerial vehicles, auxiliary power units, and distributed power generation. Other applications include thermal protection systems, dental prosthetics, fuel cells, oxygen transport membranes, radomes, and microelectromechanical systems (MEMS). In order for these high-technology ceramics to be used successfully for structural applications that push the envelope of materials capabilities, design engineers must consider that brittle materials are designed and analyzed differently than metallic materials. Unlike ductile metals, brittle materials display a stochastic strength response because of the combination of low fracture toughness and the random nature of the size, orientation, and distribution of inherent microscopic flaws. This plus the fact that the strength of a component under load may degrade over time because of slow crack growth means that a probabilistic-based life-prediction methodology must be used when the tradeoffs of failure probability, performance, and useful life are being optimized. The CARES/Life code (which was developed at the NASA Glenn Research Center) predicts the probability of ceramic components failing from spontaneous catastrophic rupture when these components are subjected to multiaxial loading and slow crack growth conditions. Enhancements to CARES/Life now allow for the component survival probability to be calculated when loading and temperature vary over time.

Nemeth, Noel N.↗

NASA NTRS2005

SiC/SiC Ceramic Matrix Composites Developed for High-Temperature Space Transportation Applications

Researchers at the NASA Glenn Research Center have been developing durable, high-temperature ceramic matrix composites (CMCs) with silicon carbide (SiC) matrices and SiC or carbon fibers for use in advanced reusable launch vehicle propulsion and airframe applications in the Next Generation Launch Technology (NGLT) Program. These CMCs weigh less and are more durable than competing metallic alloys, and they are tougher than silicon-based monolithic ceramics. Because of their high specific strength and durability at high temperatures, CMCs such as C/SiC (carbon- fiber-reinforced silicon carbide) and SiC/SiC (silicon-carbide-fiber-reinforced silicon carbide) may increase vehicle performance and safety significantly and reduce the cost of transporting payloads to orbit.

Kiser, J. Douglas↗

NASA NTRS2006

Life Limiting Behavior in Interlaminar Shear of Continuous Fiber-Reinforced Ceramic Matrix Composites at Elevated Temperatures

Interlaminar shear strength of four different fiber-reinforced ceramic matrix composites was determined with doublenotch shear test specimens as a function of test rate at elevated temperatures ranging from 1100 to 1316 C in air. Life limiting behavior, represented as interlaminar shear strength degradation with decreasing test rate, was significant for 2-D crossplied SiC/MAS-5 and 2-D plain-woven C/SiC composites, but insignificant for 2-D plain-woven SiC/SiC and 2-D woven Sylramic (Dow Corning, Midland, Michigan) SiC/SiC composites. A phenomenological, power-law delayed failure model was proposed to account for and to quantify the rate dependency of interlaminar shear strength of the composites. Additional stress rupture testing in interlaminar shear was conducted at elevated temperatures to validate the proposed model. The model was in good agreement with SiC/MAS-5 and C/SiC composites, but in poor to reasonable agreement with Sylramic SiC/SiC. Constant shear stress-rate testing was proposed as a possible means of life prediction testing methodology for ceramic matrix composites subjected to interlaminar shear at elevated temperatures when short lifetimes are expected.

Choi, Sung R.↗

NASA NTRS2006

Modeling the Stress Strain Behavior of Woven Ceramic Matrix Composites

Woven SiC fiber reinforced SiC matrix composites represent one of the most mature composite systems to date. Future components fabricated out of these woven ceramic matrix composites are expected to vary in shape, curvature, architecture, and thickness. The design of future components using woven ceramic matrix composites necessitates a modeling approach that can account for these variations which are physically controlled by local constituent contents and architecture. Research over the years supported primarily by NASA Glenn Research Center has led to the development of simple mechanistic-based models that can describe the entire stress-strain curve for composite systems fabricated with chemical vapor infiltrated matrices and melt-infiltrated matrices for a wide range of constituent content and architecture. Several examples will be presented that demonstrate the approach to modeling which incorporates a thorough understanding of the stress-dependent matrix cracking properties of the composite system.

Morscher, Gregory N.↗

NASA NTRS2006

Diffusion Bonding of Silicon Carbide Ceramics using Titanium Interlayers

Robust joining approaches for silicon carbide ceramics are critically needed to fabricate leak free joints with high temperature mechanical capability. In this study, titanium foils and physical vapor deposited (PVD) titanium coatings were used to form diffusion bonds between SiC ceramics using hot pressing. Silicon carbide substrate materials used for bonding include sintered SiC and two types of CVD SiC. Microscopy results show the formation of well adhered diffusion bonds. The bond strengths as determined from pull tests are on the order of several ksi, which is much higher than required for a proposed application. Microprobe results show the distribution of silicon, carbon, titanium, and other minor elements across the diffusion bond. Compositions of several phases formed in the joint region were identified. Potential issues of material compatibility and optimal bond formation will also be discussed.

Halbig, Michael C.↗

NASA NTRS2006

Performance Evaluations of Ceramic Wafer Seals

Future hypersonic vehicles will require high temperature, dynamic seals in advanced ramjet/scramjet engines and on the vehicle airframe to seal the perimeters of movable panels, flaps, and doors. Seal temperatures in these locations can exceed 2000 F, especially when the seals are in contact with hot ceramic matrix composite sealing surfaces. NASA Glenn Research Center is developing advanced ceramic wafer seals to meet the needs of these applications. High temperature scrub tests performed between silicon nitride wafers and carbon-silicon carbide rub surfaces revealed high friction forces and evidence of material transfer from the rub surfaces to the wafer seals. Stickage between adjacent wafers was also observed after testing. Several design changes to the wafer seals were evaluated as possible solutions to these concerns. Wafers with recessed sides were evaluated as a potential means of reducing friction between adjacent wafers. Alternative wafer materials are also being considered as a means of reducing friction between the seals and their sealing surfaces and because the baseline silicon nitride wafer material (AS800) is no longer commercially available.

Dunlap, Patrick H., Jr.↗

NASA NTRS2007

Ceramic fiber insulation impregnated with an infra-red retardant coating and method for production thereof

The invented insulation is a ceramic fiber insulation wherein the ceramic fibers are treated with a coating which contains transition metal oxides. The invented process for coating the insulation is a process of applying the transition metal oxide coating to the fibers of the insulation after the fibers have been formed into a tile or other porous body. The coating of transition metal oxide lowers the transmittance of radiation through the insulation thereby lowering the temperature of the backface of the insulation and better protecting the structure that underlies the insulation.

Zinn, Alfred A.↗

NASA NTRS2008

Monitoring Damage Accumulation in Ceramic Matrix Composites Using Electrical Resistivity

The electric resistance of woven SiC fiber reinforced SiC matrix composites were measured under tensile loading conditions. The results show that the electrical resistance is closely related to damage and that real-time information about the damage state can be obtained through monitoring of the resistance. Such self-sensing capability provides the possibility of on-board/in-situ damage detection and accurate life prediction for high-temperature ceramic matrix composites. Woven silicon carbide fiber-reinforced silicon carbide (SiC/SiC) ceramic matrix composites (CMC) possess unique properties such as high thermal conductivity, excellent creep resistance, improved toughness, and good environmental stability (oxidation resistance), making them particularly suitable for hot structure applications. In specific, CMCs could be applied to hot section components of gas turbines [1], aerojet engines [2], thermal protection systems [3], and hot control surfaces [4]. The benefits of implementing these materials include reduced cooling air requirements, lower weight, simpler component design, longer service life, and higher thrust [5]. It has been identified in NASA High Speed Research (HSR) program that the SiC/SiC CMC has the most promise for high temperature, high oxidation applications [6]. One of the critical issues in the successful application of CMCs is on-board or insitu assessment of the damage state and an accurate prediction of the remaining service life of a particular component. This is of great concern, since most CMC components envisioned for aerospace applications will be exposed to harsh environments and play a key role in the vehicle s safety. On-line health monitoring can enable prediction of remaining life; thus resulting in improved safety and reliability of structural components. Monitoring can also allow for appropriate corrections to be made in real time, therefore leading to the prevention of catastrophic failures. Most conventional nondestructive evaluation (NDE) techniques such as ultrasonic C-scan, x-ray, thermography, and eddy current are limited since they require structural components of complex geometry to be taken out of service for a substantial length of time for post-damage inspection and assessment. Furthermore, the typical NDE techniques are useful for identifying large interlaminar flaws, but insensitive to CMC materials flaws developed perpendicular to the surface under tensile creep conditions. There are techniques such as piezoelectric sensor [7,8], and optical fiber [9,10] that could be used for on-line health monitoring of CMC structures. However, these systems involve attaching an external sensor or putting special fibers in CMC composites, which would be problematic at high temperature applications.

Smith, Craig E.↗

NASA NTRS2008

Refractory Ceramic Foams for Novel Applications

Workers at NASA Ames Research center are endeavoring to develop durable, oxidation-resistant, foam thermal protection systems (TPSs) that would be suitable for covering large exterior spacecraft surfaces, would have low to moderate densities, and would have temperature capabilities comparable to those of carbon-based TPSs [reusable at 3,000 F (.1,650 C)] with application of suitable coatings. These foams may also be useful for repairing TPSs while in orbit. Moreover, on Earth as well as in outer space, these foams might be useful as catalyst supports and filters. Preceramic polymers are obvious candidates for use in making the foams in question. The use of these polymers offers advantages over processing routes followed in making conventional ceramics. Among the advantages are the ability to plastically form parts, the ability to form pyrolized ceramic materials at lower temperatures, and the ability to form high-purity microstructures having properties that can be tailored to satisfy requirements. Heretofore, preceramic polymers have been used mostly in the production of such low-dimensional products as fibers because the loss of volatiles during pyrolysis of the polymers leads to porosity and large shrinkage (in excess of 30 percent). In addition, efforts to form bulk structures from preceramic polymers have resulted in severe cracking during pyrolysis. However, because the foams in question would consist of networks of thin struts (in contradistinction to nonporous dense solids), these foams are ideal candidates for processing along a preceramic-polymer route.

Stackpoole, M.↗

NASA NTRS2009

Ballistic Performance of Porous Ceramic Thermal Protection Systems at 9 km/s

Porous-ceramic, thermal-protection-systems are used heavily in current reentry vehicles like the Orbiter, and they are currently being proposed for the next generation of manned spacecraft, Orion. These materials insulate the structural components and sensitive electronic components of a spacecraft against the intense thermal environments of atmospheric reentry. Furthermore, these materials are also highly exposed to space environmental hazards like meteoroid and orbital debris impacts. This paper discusses recent impact testing up to 9 km/s on ceramic tiles similar to those used on the Orbiter. These tiles have a porous-batting of nominally 8 lb/cubic ft alumina-fiber-enhanced-thermal-barrier (AETB8) insulating material coated with a damage-resistant, toughened-unipiece-fibrous-insulation (TUFI) layer.

Miller, Joshua E.↗

NASA NTRS2009

Ceramic Fiber Structures for Cryogenic Load-Bearing Applications

This invention is intended for use as a load-bearing device under cryogenic temperatures and/or abrasive conditions (i.e., during missions to the Moon). The innovation consists of small-diameter, ceramic fibers that are woven or braided into devices like ropes, belts, tracks, or cables. The fibers can be formed from a variety of ceramic materials like silicon carbide, carbon, aluminosilicate, or aluminum oxide. The fiber architecture of the weave or braid is determined by both the fiber properties and the mechanical requirements of the application. A variety of weave or braid architectures is possible for this application. Thickness of load-bearing devices can be achieved by using either a 3D woven structure, or a layered, 2D structure. For the prototype device, a belt approximately 0.10 in. (0.25 cm) thick, and 3.0 in. (7.6 cm) wide was formed by layering and stitching a 2D aluminosilicate fiber weave.

Jaskowiak, Martha H.↗

NASA NTRS2009

Assessment of the State of the Art of Ultra High Temperature Ceramics

Ultra High Temperature Ceramics (UHTCs) are a family of materials that includes the borides, carbides and nitrides of hafnium-, zirconium- and titanium-based systems. UHTCs are famous for possessing some of the highest melting points of known materials. In addition, they are very hard, have good wear resistance, mechanical strength, and relatively high thermal conductivities (compared to other ceramic materials). Because of these attributes, UHTCs are ideal for thermal protection systems, especially those that require chemical and structural stability at extremely high operating temperatures. UHTCs have the potential to revolutionize the aerospace industry by enabling the development of sharp hypersonic vehicles or atmospheric entry probes capable of the most extreme entry conditions.

Johnson, Sylvia↗

NASA NTRS2010

Review of Leading Approaches for Mitigating Hypersonic Vehicle Communications Blackout and a Method of Ceramic Particulate Injection Via Cathode Spot Arcs for Blackout Mitigation

Vehicles flying at hypersonic velocities within the atmosphere become enveloped in a "plasma sheath" that prevents radio communication, telemetry, and most importantly, GPS signal reception for navigation. This radio "blackout" period has been a problem since the dawn of the manned space program and was an especially significant hindrance during the days of the Apollo missions. An appropriate mitigation method must allow for spacecraft to ground control and ground control to spacecraft communications through the reentry plasma sheath. Many mitigation techniques have been proposed, including but not limited to, aerodynamic shaping, magnetic windows, and liquid injection. The research performed on these mitigation techniques over the years will be reviewed and summarized, along with the advantages and obstacles that each technique will need to overcome to be practically implemented. A unique approach for mitigating the blackout communications problem is presented herein along with research results associated with this method. The novel method involves the injection of ceramic metal-oxide particulate into a simulated reentry plasma to quench the reentry plasma. Injection of the solid ceramic particulates is achieved by entrainment within induced, energetic cathode spot flows.

Gillman, Eric D.↗

NASA NTRS2010

Thin Film Heat Flux Sensor Development for Ceramic Matrix Composite (CMC) Systems

The NASA Glenn Research Center (GRC) has an on-going effort for developing high temperature thin film sensors for advanced turbine engine components. Stable, high temperature thin film ceramic thermocouples have been demonstrated in the lab, and novel methods of fabricating sensors have been developed. To fabricate thin film heat flux sensors for Ceramic Matrix Composite (CMC) systems, the rough and porous nature of the CMC system posed a significant challenge for patterning the fine features required. The status of the effort to develop thin film heat flux sensors specifically for use on silicon carbide (SiC) CMC systems with these new technologies is described.

Wrbanek, John D.↗

NASA NTRS2010

Oxidation Characterization of Hafnium-Based Ceramics Fabricated by Hot Pressing and Electric Field-Assisted Sintering

Ceramic borides, such as hafnium diboride (HfB2) and zirconium diboride (ZrB2), are members of a family of materials with extremely high melting temperatures referred to as Ultra High Temperature Ceramics (UHTCs). UHTCs constitute a class of promising materials for use in high temperature applications, such as sharp leading edges on future-generation hypersonic flight vehicles, because of their high melting points. The controlled development of microstructure has become important to the processing of UHTCs, with the prospect of improving their mechanical and thermal properties. The improved oxidation resistance of HfB2 has also become important if this material is to be successfully used at temperatures above 2000 C. Furthermore, the use of UHTCs on the leading edges of vehicles traveling at hypersonic speeds will mean exposure to a mixed oxidation environment comprised of both molecular and atomic oxygen. The current study has investigated the high-temperature oxidation behavior of HfB2-based materials in a pure O2 environment, as well as in environments containing different levels of dissociated oxygen (O/O2). Materials were processed by two techniques: conventional hot pressing (HP) and electric field-assisted sintering (FAS). Their oxidation behavior was evaluated in both a tube furnace at 1250 C for 3 hours and in a simulated re-entry environment in the Advanced Heating Facility (AHF) arcjet at NASA Ames Research Center, during a 10-minute exposure to a cold wall heat flux of 250W/sq cm and stagnation pressure of 0.1-0.2 atm. The microstructure of the different materials was characterized before and after oxidation using scanning electron microscopy (SEM).

Gasch, Matt↗

NASA NTRS2010

High efficiency tantalum-based ceramic composite structures

Tantalum-based ceramics are suitable for use in thermal protection systems. These composite structures have high efficiency surfaces (low catalytic efficiency and high emittance), thereby reducing heat flux to a spacecraft during planetary re-entry. These ceramics contain tantalum disilicide, molybdenum disilicide and borosilicate glass. The components are milled, along with a processing aid, then applied to a surface of a porous substrate, such as a fibrous silica or carbon substrate. Following application, the coating is then sintered on the substrate. The composite structure is substantially impervious to hot gas penetration and capable of surviving high heat fluxes at temperatures approaching 3000.degree. F. and above.

Stewart, David A.↗