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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.
Polymer infiltration of a rigidized preform, followed by pyrolysis to convert the polymer to a ceramic, potentially offers a lower cost alternative to CVD. It also offers more moderate temperature requirements than melt infiltration approaches, which should minimize potential fiber damage during processing. However, polymer infiltration and pyrolysis results in a more microcracked matrix. Preliminary mechanical property characterization, including elevated temperature (1204 C) tensile, 500 h stress rupture behavior and low cycle fatigue, was conducted on Hi-Nicalon (TM)/Si-C-(O) composites having a dual layer BN/SiC interface and a matrix derived by impregnation and pyrolysis of allylhydridopolycarbosilane (AHPCS). Microstructural evaluation of failure surfaces and of polished transverse and longitudinal cross sections of the failed specimens was used to identify predominant failure mechanisms. In stress rupture testing at 1093 C, the failure was interface dominated, while at 1204 C in both stress rupture and two hour hold/fatigue tests failure was matrix dominated, resulting in specimen delamination.
A ceramic composite thin film or layer includes individual graphene oxide and/or electrically conductive graphene sheets dispersed in a ceramic (e.g. silica) matrix. The thin film or layer can be electrically conductive film or layer depending the amount of graphene sheets present. The composite films or layers are transparent, chemically inert and compatible with both glass and hydrophilic SiOx/silicon substrates. The composite film or layer can be produced by making a suspension of graphene oxide sheet fragments, introducing a silica-precursor or silica to the suspension to form a sol, depositing the sol on a substrate as thin film or layer, at least partially reducing the graphene oxide sheets to conductive graphene sheets, and thermally consolidating the thin film or layer to form a silica matrix in which the graphene oxide and/or graphene sheets are dispersed.
A ceramic reusable, externally applied composite thermal protection system (TPS) is proposed. The system functions by utilizing a ceramic/ceramic upper shell structure which effectively separates its primary functions as a thermal insulator and as a load carrier to transmit loads to the cold structure. The composite tile system also prevents impact damage to the atmospheric entry vehicle thermal protection system. The composite tile comprises a structurally strong upper ceramic/ceramic shell manufactured from ceramic fibers and ceramic matrix meeting the thermal and structural requirements of a tile used on a re-entry aerospace vehicle. In addition, a lightweight high temperature ceramic lower temperature base tile is used. The upper shell and lower tile are attached by means effective to withstand the extreme temperatures (3000 to 3200F) and stress conditions. The composite tile may include one or more layers of variable density rigid or flexible thermal insulation. The assembly of the overall tile is facilitated by two or more locking mechanisms on opposing sides of the overall tile assembly. The assembly may occur subsequent to the installation of the lower shell tile on the spacecraft structural skin.
Composite Because of their high specific stiffness and strength at elevated temperatures, continuously reinforced metal matrix composites (MMC's) are under consideration for a future generation of aeropropulsion systems. Since components in aeropropulsion systems experience substantial cyclic thermal and mechanical loads, the fatigue behavior of MMC's is of great interest. Almost without exception, previous investigations of the fatigue behavior of MMC's have been conducted in a tension-tension, load-controlled mode. This has been due to the fact that available material is typically less than 2.5-mm thick and, therefore, unable to withstand high compressive loads without buckling. Since one possible use of MMC's is in aircraft skins, this type of testing mode may be appropriate. However, unlike aircraft skins, most engine components are thick. In addition, the transient thermal gradients experienced in an aircraft engine will impose tension-compression loading on engine components, requiring designers to understand how the MMC will behave under fully reversed loading conditions. The increased thickness of the MMC may also affect the fatigue life. Traditionally, low-cycle fatigue (LCF) tests on MMC's have been performed in load control. For monolithic alloys, low-cycle fatigue tests are more typically performed in strain control. Two reasons justify this choice: (1) the critical volume from which cracks initiate and grow is generally small and elastically constrained by the larger surrounding volume of material, and (2) load-controlled, low-cycle fatigue tests of monolithics invariably lead to unconstrained ratcheting and localized necking--an undesired material response because the failure mechanism is far more severe than, and unrelated to, the fatigue mechanism being studied. It is unknown if this is the proper approach to composite testing. However, there is a lack of strain-controlled data on which to base any decisions. Consequently, this study addresses the isothermal, LCF behavior of a [0]_32 MMC tested under strain- and load-controlled conditions for both zero-tension and tension-compression loading conditions. These tests were run at 427 C on thick specimens of SiC-reinforced Ti-15-3. For the fully-reversed tests, no difference was observed in the lives between the load- and strain-controlled tests. However, for the zero-tension tests, the strain-controlled tests had longer lives by a factor of 3 in comparison to the load-controlled tests. This was due to the fact that under strain-control the specimens cyclically softened, reducing the cracking potential. In contrast, the load-controlled tests ratcheted toward larger tensile strains leading to an eventual overload of the fibers. Fatigue tests revealed that specimens tested under fully-reversed conditions had lives approximately an order of magnitude longer than for those specimens tested under zero tension. When examined on a strain-range basis, the fully reversed specimens had similar, but still shorter lives than those of the unreinforced matrix material. However, the composite had a strain limitation at short lives because of the limited strain capacity of the brittle ceramic fiber. The composite also suffered at very high lives because of the lack of an apparent fatigue limit in comparison to the unreinforced matrix. The value of adding fibers to the matrix is apparent when the fatigue lives are plotted as a function of stress range. Here, the composite is far superior to the unreinforced matrix because of the additional load-carrying capacity of the fibers.
This paper describes the tensile behavior of high-temperature composite materials containing continuous Nicalon ceramic fiber reinforcement and glass and glass/ceramic matrices. The longitudinal properties of these materials can approach theoretical expectations for brittle matrix composites, failing at a strength and ultimate strain level consistent with those of the fibers. The brittle, high-modulus matrices result in a nonlinear stress-strain curve due to the onset of stable matrix cracking at 10 to 30 percent of the fiber strain to failure, and at strains below this range in off-axis plies. Current fibers and matrices can provide attractive properties well above 1000 C, but composites experience embrittlement in oxidizing atmospheres at 800 to 1000 C due to oxidation of a carbon interface reaction layer.The oxidation effect greatly increases the interface bond strength, causing composite embrittlement.
For propulsion related applications, materials must be able to demonstrate excellent ablation and oxidation resistance at temperature approaching 3500'C, adequate load bearing capabilities, non-catastrophic failure modes, and ability to withstand transient thermal shock. A potential list of propulsion-material property requirements includes, low density, high elastic modulus, low thermal-expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. In many cases, they will also need to be able to be joined, survive thermal cycling and multi-axial stress states, and for reusable applications, the materials must maintain the above attributes after prolonged exposure to extremely harsh chemical environments. The final and possibly most important attribute for these materials are the need to be lower cost and readily available in large quantities. Recently, Advanced Ceramics Research, Inc. (ACR) has developed low cost, flexible- manufacturing processes for Zr & Hf-based carbon fiber reinforced composites, materials with good oxidation and ablation resistance up to 3500 C. This process, called Continuous Composite Co-extrusion (C(sup 3)), incorporates carbon fibers to fabricate 'in-situ' carbide and boride-matrix/carbon fiber composites. This is a variation of ACR's manufacturing process for low-cost structural ceramic materials called Fibrous Monoliths With carbon fiber reinforcements. Fibrous Monolithic materials have a distinct fibrous texture, consist of intertwined cells of a primary phase, separated by cell boundaries of a tailored secondary phase and show very high fracture energies, damage tolerance, and graceful failure. Since they are monolithic powder based composites-, they can be manufactured by conventional powder processing techniques using inexpensive raw materials. This combination of high performance and low cost is a breakthrough that could enable wider application of ceramics in high temperature applications. Typical volume fractions of the two phases are 80 to 95% for the cell phase and 5 to 20% for the interpenetrating cell boundary phase. ACR is currently developing an innovative solid freeform form fabrication (SFF) approach to produce Hf and Zr based ceramic composite components reinforced with continuous carbon fiber tows for critical structural components such as tubes and blisks. The process is simple, robust and will be widely applicable to a number of material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The current process is being developed in collaboration with UD-CCM. The paper will detail the freeform fabrication process to create low-cost ceramic fiber reinforced composites for high-temperature applications. The results of mechanical properties and microstructural characterization will be presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts for propulsion applications at an order of magnitude lower cost than current CVI and PIP process.
For propulsion related applications, materials must be able to demonstrate excellent ablation and oxidation resistance at temperature approaching 3500 C, adequate load bearing capabilities, non-catastrophic failure modes, and ability to withstand transient thermal shock. A potential list of propulsion-material property requirements includes, low density, high elastic modulus, low thermal-expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. In many cases, they will also need to be able to be joined, survive thermal cycling and multi-axial stress states, and for reusable applications, the materials must maintain the above attributes after prolonged exposure to extremely harsh chemical environments. The final and possibly most important attribute for these materials are the need to be lower cost and readily available in large quantities. Recently, Advanced Ceramics Research, Inc. (ACR) has developed low cost, flexible-manufacturing processes for Zr & Hf-based carbon fiber reinforced composites, materials with good oxidation and ablation resistance up to 3500 C. This process, called Continuous Composite Co-extrusion (C(sup 3)), incorporates carbon fibers to fabricate 'in-situ' carbide and boride-matrix/carbon fiber composites. M is a variation of ACR's manufacturing process for low-cost structural ceramic materials called Fibrous Monoliths with carbon fiber reinforcements. Fibrous Monolithic materials have a distinct fibrous texture, consist of intertwined cells of a primary phase, separated by cell boundaries of a tailored secondary phase and show very high fracture energies, damage tolerance, and graceful failure. Since they are monolithic powder based composites; they can be manufactured by conventional powder processing techniques using inexpensive raw materials. This combination of high performance and low cost is a breakthrough that could enable wider application of ceramics in high temperature applications. Typical volume fractions of the two phases are 80 to 95% for the cell phase and 5 to 20% for the interpenetrating cell boundary phase. ACR is currently developing an innovative solid freeform form fabrication (SFF) approach to produce Hf and Zr based ceramic composite components reinforced with continuous carbon fiber tows for critical structural components such as tubes and blisks. The process is simple, robust and will be widely applicable to a number of material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The current process is being developed in collaboration with UD-CCM. The paper will detail the freeform fabrication process to create low-cost ceramic fiber reinforced composites for high-temperature applications. The results of mechanical properties and microstructural characterization will be presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts for propulsion applications at an order of magnitude lower cost than current CVI and PIP processes.
Metal-oxide composites are commonly used in high temperature environments for their thermal stability and high melting points. Commonly employed with refractory oxides or carbides such as ZrC and HfC, these materials may be improved with the use of a low density, high melting point ceramic such as CeO2. In this work, the consolidation of W-CeO2 metal matrix composites in the high CeO2 concentration regime is explored. The CeO2 concentrations of 50, 33, and 25 wt.%, the CeO2 particle size from nanometer to micrometer, and various hot isostatic pressing temperatures are investigated. Decreasing the CeO2 concentration is observed to increase the composite density and increase the Vickers hardness. The CeO2 oxidation state is observed to be a combination of Ce3+ and Ce4+, which is hypothesized to contribute to the porosity of the composites. The hardness of the metal-oxide composite can be improved more than 2.5 times compared to pure W processed by the same route. This work offers processing guidelines for further consolation of oxide-doped W composites.
In spite of great improvements in accuracy through the use of computers, design methods, which can be equally critical in establishing the commercial success of a material, have been treated as afterthoughts. Early investment in design and development technologies can easily reduce manufacturing costs later in the product cycle. To avoid lengthy product development times for ceramic composites, funding agencies for materials research must commit resources to support design and development technologies early in the material life cycle. These technologies need not focus on designing the material, rather, the technology must focus on designing with the material, i. e., developing methods to design components fabricated from the new material. Thus a basic tenet that motivated this research effort is that a persistent need exists for improvements in the analysis of components fabricated from CMC material systems. From an aerospace design engineer's perspective the new generation of ceramic composites offers a significant potential for raising the thrust/weight ratio and reducing NOx emissions of gas turbine engines. Continuous ceramic fiber composites exhibit an increase in work of fracture, which allows for 'graceful' rather than catastrophic failure. When loaded in the fiber direction, these composites retain substantial strength capacity beyond the initiation of transverse matrix cracking despite the fact that neither of its constituents would exhibit such behavior if tested alone. As additional load is applied beyond first matrix cracking, the matrix tends to break in a series of cracks bridged by the ceramic fibers. Thus any additional load is born increasingly by the fibers until the ultimate strength of the composite is reached. Establishing design protocols that enable the engineer to analyze and predict this type of behavior in ceramic composites was the general goal of this project.
Uranium nitride has been under consideration at NASA and the Department of Energy for nuclear thermal propulsion applications intended for deep space exploration vehicles. It is critical to the success of the technology development that the behavior of the fuel system is properly characterized in operational environments. This body of work fabricated ceramic metal composites consisting of uranium ceramic fuel in a molybdenum and molybdenum–tungsten metal matrix, both with and without an exterior molybdenum barrier. Specimens were introduced to a high temperature hydrogen environment and characterized through x-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy to identify characteristic changes. A portion of the specimens was fabricated with a 1.27 mm thick molybdenum barrier in order to isolate the material from the hydrogen environment. Instability of the uranium nitride occurred as low as 2073 K, leading to aggressive instability approaching 2658 K. Carbon reactions with the metal matrix were observed as well as alloying between the uranium and metal matrix constituents. The liquid uranium resulting from the instability of the uranium nitride was observed to attack the grain boundaries of the refractory metal, resulting in the formation of a liquid uranium molybdenum eutectic melt. Specimens encased in a barrier experienced similar results. The authors conclude this is a significant challenge to applications of this cermet at these temperatures. Alternate configurations with resilient hermetic seals or lower temperature applications such as power reactors may have more success.
Ceramic joining is recognized as one of the enabling technologies for the successful utilization of silicon carbide-based monolithic ceramic and fiber reinforced composite components in a number of demanding and high temperature applications in aerospace and ground-based systems. An affordable, robust ceramic joining technology (ARCJoinT) for joining of silicon carbide-based ceramics and fiber reinforced composites has been developed. This technique is capable of producing joints with tailorable thickness and composition. A wide variety of silicon carbide-based ceramics and composites, in different shapes and sizes, have been joined using this technique. The room and high temperature mechanical properties and fractography of ceramic joints have been reported. In monolithic silicon carbide ceramics, these joints maintain their mechanical strength up to 1350 C in air. There is no change in the mechanical strength of joints in silicon carbide matrix composites up to 1200 C in air. In composites, simple butt joints yield only about 20% of the ultimate strength of the parent materials. This technology is suitable for the joining of large and complex shaped ceramic and composite components, and with certain modifications, can be applied to repair of ceramic components damaged in service.
It is evident that for proper micromechanical analysis of ceramic composites, one needs to use a numerical method that is capable of idealizing the individual fibers or individual bundles of fibers embedded within a three-dimensional ceramic matrix. The analysis must be able to account for high stress or temperature gradients from diffusion of stress or temperature from the fiber to the ceramic matrix and allow for interaction between the fibers through the ceramic matrix. The analysis must be sophisticated enough to deal with the failure of fibers described by a series of increasingly sophisticated constitutive models. Finally, the analysis must deal with micromechanical modeling of the composite under nonlinear thermal and dynamic loading. This report details progress made towards the development of a boundary element code designed for the micromechanical studies of an advanced ceramic composite. Additional effort has been made in generalizing the implementation to allow the program to be applicable to real problems in the aerospace industry.
Polymer-derived ceramics (PDCs) remain at the forefront of research for a variety of applications including ultra-high-temperature ceramics, energy storage and functional coatings. Despite their wide use, questions remain about the complex structural transition from polymer to ceramic and how local structure influences the final microstructure and resulting properties. This is further complicated when nanofillers are introduced to tailor structural and functional properties, as nanoparticle surfaces can interact with the matrix and influence the resulting structure. The inclusion of crystalline nanofiller produces a mixed crystalline–amorphous composite, which poses characterization challenges. With this study, we aim to address these challenges with a local-scale structural study that probes changes in a polysiloxane matrix with incorporated copper nanofiller. Composites were processed at three unique temperatures to capture mixing, pyrolysis and initial crystallization stages for the pre-ceramic polymer. We observed the evolution of the nanofiller with electron microscopy and applied synchrotron X-ray diffraction with differential pair distribution function (d-PDF) analysis to monitor changes in the matrix's local structure and interactions with the nanofiller. The application of the d-PDF to PDC materials is novel and informs future studies to understand interfacial interactions between nanofiller and matrix throughout PDC processing.
An analytical study was conducted to assess the feasibility of and benefits derived from the use of high temperature composite materials in aircraft turbine engine combustor liners. The study included a survey and screening of the properties of three candidate composite materials including tungsten reinforced superalloys, carbon-carbon and silicon carbide (SiC) fibers reinforcing a ceramic matrix of lithium aluminosilicate (LAS). The SiC-LAS material was selected as offering the greatest near term potential primarily on the basis of high temperature capability. A limited experimental investigation was conducted to quantify some of the more critical mechanical properties of the SiC-LAS composite having a multidirection 0/45/-45/90 deg fiber orientation favored for the combustor linear application. Rigorous cyclic thermal tests demonstrated that SiC-LAS was extremely resistant to the thermal fatigue mechanisms that usually limit the life of metallic combustor liners. A thermal design study led to the definition of a composite liner concept that incorporated film cooled SiC-LAS shingles mounted on a Hastelloy X shell. With coolant fluxes consistent with the most advanced metallic liner technology, the calculated hot surface temperatures of the shingles were within the apparent near term capability of the material. Structural analyses indicated that the stresses in the composite panels were low, primarily because of the low coefficient of expansion of the material and it was concluded that the dominant failure mode of the liner would be an as yet unidentified deterioration of the composite from prolonged exposure to high temperature. An economic study, based on a medium thrust size commercial aircraft engine, indicated that the SiC-LAS combustor liner would weigh 22.8N (11.27 lb) less and cost less to manufacture than advanced metallic liner concepts intended for use in the late 1980's.
An evaluation is made of the state-of-the-art and foreseeable development prospects in high temperature engineering materials applicable to advanced heat engines and other aerothermodynamically affected structures. Attention is given to monocrystal- and microcrystal-producing metal solidification processes, soft oxide and chemically stable fluoride high temperature solid lubricants, polyimide and other high temperature polymers for propulsion system applications, high strength/toughness ceramics for heat engine structural components, thermal barrier coatings, and metal-matrix composites employing refractory matrices as well as reinforcing fibers.
From the company that brought the world an integral heating and cooling food service system after originally developing it for NASA's Apollo Program, comes yet another orbital offshoot: a product that can be as thin as paper and as strong as steel. Nextel Ceramic Textiles and Composites from 3M Company offer space-age protection and innovative solutions for hot situations, ranging from NASA to NASCAR. With superior thermal protection, Nextel fabrics, tape, and sleevings outperform other high temperature textiles such as aramids, carbon, glass, and quartz, permitting engineers and manufacturers to handle applications up to 2,500 F (1,371 C). The stiffness and strength of Nextel Continuous Ceramic Fibers make them a great match for improving the rigidity of aluminum in metal matrix composites. Moreover, the fibers demonstrate low shrinkage at operating temperatures, which allow for the manufacturing of a dimensionally stable product. These novel fibers also offer excellent chemical resistance, low thermal conductivity, thermal shock resistance, low porosity, and unique electrical properties.
The present research effort was undertaken to develop a new generation of SiC fiber- reinforced engineered matrix composites (EMCs) with sufficient high temperature plasticity to reduce crack propagation and self-healing capabilities to fill surface-connected cracks to prevent the oxygen ingress to the fibers. A matrix engineered with these capabilities is expected to increase the load bearing capabilities of SiCSiC CMCs at high temperatures. Several matrix compositions were designed to match the coefficient of thermal expansion (CTE) of the SiC fibers using a rule of mixture (ROM) approach. The CTE values of these matrices were determined and it was demonstrated that they were generally in good agreement with that of monolithic SiC between room temperature and 1525 K. The parameters to hot press the powders were optimized, and specimens were fabricated for determining bend strength, CTE, oxidation and microstructural characteristics of the engineered matrices. The oxidation tests revealed that some of the matrices exhibited catastrophic oxidation, and therefore, these were eliminated from further consideration. Two promising compositions were down selected based on these results for further development. Four-point bend tests were conducted on these two promising matrices between room temperature and 1698 K. Although theses matrices were brittle and failed at low stresses at room temperature, they exhibited high temperature ductility and higher stresses at the higher temperatures. The effects of different additives on the self-healing capabilities of these matrices were investigated. The results of preliminary studies conducted to slurry and melt infiltration trials with CrSi2 are described.