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NASA NTRS2001

Solid Freeform Fabrication of Continuous Fiber Reinforced Composites for Propulsion Applications

Monolithic ceramics lack the fracture toughness necessary to be considered for propulsion related applications. To be used for such applications, materials must possess low density, high elastic modulus, a low thermal expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. They will in many cases also be required to possess the ability to be joined, to 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 attributes for these materials are the need to be of low cost and readily available in large quantities.

Vaidyanathan, R.↗

NASA NTRS2000

Solid Freeform Fabrication of Continuous Fiber Reinforced Composites for Propulsion Applications

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.

Vaidyanathan, R.↗

NASA NTRS1989

Ceramic heat pipe wick

A wick for use in a capillary loop pump heat pipe is disclosed. The wick material is an essentially uniformly porous, permeable, open-cell, silicon dioxide/aluminum oxide inorganic ceramic foam having a silica fiber ratio, by weight, of about 78 to 22, respectively, a density of 6 lbs/cu ft, and an average pore size of less than 5 microns. A representative material having these characteristics is Lockheed Missile and Space Company, Inc.'s HTP 6-22. This material is fully compatible with the freons and anhydrous ammonia and allows for the use of these very efficient working fluids, and others, in capillary loops.

Seidenberg, Benjamin↗

NASA NTRS1994

Development of processing techniques for advanced thermal protection materials

The effort, which was focused on the research and development of advanced materials for use in Thermal Protection Systems (TPS), has involved chemical and physical testing of refractory ceramic tiles, fabrics, threads and fibers. This testing has included determination of the optical properties, thermal shock resistance, high temperature dimensional stability, and tolerance to environmental stresses. Materials have also been tested in the Arc Jet 2 x 9 Turbulent Duct Facility (TDF), the 1 atmosphere Radiant Heat Cycler, and the Mini-Wind Tunnel Facility (MWTF). A significant part of the effort hitherto has gone towards modifying and upgrading the test facilities so that meaningful tests can be carried out. Another important effort during this period has been the creation of a materials database. Computer systems administration and support have also been provided. These are described in greater detail below.

Selvaduray, Guna S.↗

NASA NTRS1998

Fiber Optic Cable Feedthrough and Sealing

A novel fiberoptic hermetic bulkhead feedthrough has been developed which will offer cryogenic sealing at leak rates of 10(exp -11) cc/sec helium. This feedthrough was developed for NASA in response to needs for a hermetically sealed feedthrough which could withstand a range of temperatures from low cryogenic (-196 C), due to liquid fuels and oxidizers, to high temperatures (+200 C) encountered in the proximity of combustion gasses. The development effort will be reported from conceptual design of single and multi-channel feedthrough units with single interconnection interfaces to units with double-ended interconnection interfaces. Various combinations of fiber/buffers are reported with recommendations based on test results. A comprehensive series of environmental and mechanical tests were performed to evaluate the feedthroughs in adverse conditions. Test results are reported including insertion loss, salt spray, sinusoidal vibration, random vibration, mechanical shock, thermal shock and humidity. A second set of feedthrough units was exposed to 3 different types of radiation. Optical transmittance changes during the tests were monitored and leak rate testing was done after each test. State-of-the-art technology in optical fiber feedthroughs constructed with polycrystalline ceramic is presented.

Fan, Robert J.↗

NASA NTRS1999

Method of Fabricating Chopped-Fiber Composite Piston

A three-dimensional piston molding is fabricated from a mixture of chopped, carbon tow filaments of variable length, which are prepregged with carbonaceous organic resins and/or pitches and molded by conventional molding processes into a near net shape, to form a carbon-fiber reinforced organic-matrix composite part. Continuous reinforcement in the form of carbon-carbon composite tapes or pieces of fabric can be also laid in the mold before or during the charging of the mold with the chopped-fiber mixture, to enhance the strength in the crown and wrist-pin areas. The molded chopped-fiber reinforced organic-matrix composite parts are then pyrolized in an inert atmosphere, to convert the organic matrix materials to carbon. These pyrolized parts are then densified by reimpregnation with resins or pitches, which are subsequently carbonized. Densification is also accomplished by direct infiltration with carbon by vapor deposition processes. Once the desired density has been achieved, the piston molds are machined to final piston dimensions, and piston ring grooves are added. To prevent oxidation and/or to seal the piston surface or near surface, the chopped-fiber piston is coated with ceramic and/or metallic sealants: and/or coated with a catalyst.

Rivers, H. Kevin↗

NASA NTRS2001

Solid Free-Form Fabrication of Continuous Fiber Reinforced Composites for Propulsion Application

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.

Vaidyanathan, R.↗

NASA NTRS1985

High temperature metal and ceramic composites

The Materials Division at NASA Lewis is engaged in research and development efforts on behalf of fiber-reinforced composite materials that are lighter, stiffer, and more structurally reliable than conventional monolithic alloys and ceramics in applications that range from the cryogenic to the refractory. Attention is presently given to metal matrix composites, in which high performance depends on stiff, strong and thermally stable large diameter fibers, with chemically stable interfacial bonding and good coefficient of thermal expansion matching between fibers and matrices, and to ceramic matrix composites, in which intermediate strength interfacial bonds must allow cracks to propagate through the matrix only, while retaining good load transfer characteristics between fiber and matrix.

Signorelli, R. A.↗

NASA NTRS1968

Reinforced thermal-shock resistant ceramics

Composite material, made by dispersing short tungsten-rhenium fibers randomly throughout zirconium oxide, is highly resistant to oxidizing environments at temperatures above 2000 degrees F. This reinforced ceramic is also thermal stress resistant.

Crump, D. N.↗

NASA NTRS1998

Modeling the Mechanical Behavior of Ceramic Matrix Composite Materials

Ceramic matrix composites are ceramic materials, such as SiC, that have been reinforced by high strength fibers, such as carbon. Designers are interested in using ceramic matrix composites because they have the capability of withstanding significant loads while at relatively high temperatures (in excess of 1,000 C). Ceramic matrix composites retain the ceramic materials ability to withstand high temperatures, but also possess a much greater ductility and toughness. Their high strength and medium toughness is what makes them of so much interest to the aerospace community. This work concentrated on two different tasks. The first task was to do an extensive literature search into the mechanical behavior of ceramic matrix composite materials. This report contains the results of this task. The second task was to use this understanding to help interpret the ceramic matrix composite mechanical test results that had already been obtained by NASA. Since the specific details of these test results are subject to the International Traffic in Arms Regulations (ITAR), they are reported in a separate document (Jordan, 1997).

Jordan, William↗

NASA NTRS1985

Strain isolated ceramic coatings

Plasma sprayed ceramic coatings are used in gas turbine engines to improve component temperature capability and cooling air efficiency. A compliant metal fiber strain isolator between a plasma sprayed ceramic coating and a metal substrate improves ceramic durability while allowing thicker coatings for better insulation. Development of strain isolated coatings has concentrated on design and fabrication of coatings and coating evaluation via thermal shock testing. In thermal shock testing, five types of failure are possible: buckling failure im compression on heat up, bimetal type failure, isothermal expansion mismatch failure, mudflat cracking during cool down, and long term fatigue. A primary failure mode for thermally cycled coatings is designated bimetal type failure. Bimetal failure is tensile failure in the ceramic near the ceramic-metal interface. One of the significant benefits of the strain isolator is an insulating layer protecting the metal substrate from heat deformation and thereby preventing bimetal type failure.

Tolokan, R. P.↗

NASA NTRS1986

Polymer precursors for ceramic matrix composites

The synthesis and characterization of a polycyclohexasilane is reported. Because of its cyclic structure, it is anticipated that this polymer might serve as a precursor to SIC having a high char yield with little rearrangement to form small, volatile cyclic silanes, and, as such, would be of interest as a precursor to SiC composite matrices and fibers, or as a binder in ceramic processing. Several approaches to the synthesis of a bifunctional cyclic monomer were attempted; the most successful of these was metal coupling of PhMeSiCl2 and Me2SiCl2. The procedure gives six-membered ring compounds with all degrees of phenyl substitution, from none to hexaphenyl. The compounds with from 0-2 groups were isolated and characterized. The fraction with degree of phenyl substitution equal to 2, a mixture of cis and trans 1,2-; 1,3-; and 1,4 isomers, was isolated in 32 percent yield. Pure 1,4 diphenyldecamethylcyclohexasilane was isolated from the mixed diphenyl compounds and characterized. Diphenyldecamethylcyclohexasilanes were dephenylated to dichlorodecamethylcyclohexasilanes by treating with H2SO4.NH4Cl in benzene. The latter were purified and polymerized by reacting with sodium in toluene. The polymers were characterized by HPGPC, elemental analysis, proton NMR, and IR. Thermogravimetric analyses were carried out on the polymers. As the yield of residual SiC was low, polymers were heat treated to increase the residual char yield. As high as 51.52 percent residual char yield was obtained in one case.

Litt, M. H.↗

NASA NTRS2018

Importance of Measuring SiC Fiber Diameter Prior to Conducting Fiber Stress Rupture / Creep Tests?

A very significant amount of SiC fiber creep / stress rupture data has been generated and reported in the past by various researchers. Due to the difficulty of measuring fiber diameter and the amount of time required to make accurate measurements, researchers have quite often used an accepted average diameter value (which is fiber type-dependent) when determining the load that will be applied to a fiber to generate a specific stress during testing. Of course, this approach has less of an effect on data scatter when the individual fibers in a tow have very similar diameters (minimal fiber-to-fiber variation in diameter). NASA GRC has begun using a laser fiber diameter measurement system, and we are considering eventually characterizing each SiC fiber prior to testing in creep/stressed oxidation. The laser system will be described in this presentation, as well as examples of fiber diameter data obtained in the past at AFRL. We are currently discussing the merits of using an average diameter in testing/data analysis vs. using a measured or "known" diameter. Information about our current intermediate temperature SiC fiber stress rupture testing will also be provided.

ceramic matrix composites↗

NASA NTRS2005

New Fiber Reinforced Waterless Concrete for Extraterrestrial Structural Applications

Commercial use of sulfur concrete on Earth is well established, particularly in corrosive, e.g., acid and salt, environments. Having found troilite (FeS) on the Moon raises the question of using extracted sulfur as a lunar construction mate: iii an attractive alternative to conventional concrete as it does not require water For the purpose of this paper it is assumed that lunar ore is mined, refined, and the raw sulfur processed with appropriate lunar regolith to form, for example, brick and beam elements. Glass fibers produced from regolith were used as a reinforcement to improve the mechanical properties of the sulfur concrete. Glass fibers and glass rebar were produced by melting the lunar regolith simulant. Lunar regolith stimulant was melted in a 25 cc Pt-Rh crucible in a Sybron Thermoline 46100 high temperature MoSi2 furnace at melting temperatures of 1450 to 1600G. The glass melt wets the ceramic rod and long continuous glass fibers were easily hand drawn. The glass fibers were immediately coated with a protective polymer to maintain the mechanical strength. The viability of sulfur concrete as a construction material for extraterrestrial application is presented. The mechanical properties of the glass fiber reinforced sulfur concrete were investigated.

Toutanji, H.↗

NASA NTRS1985

Fabrication of Slender Struts for Deployable Antennas

High moduli of elasticity potentially achievable. Suited for application in large diameter antennas on orbiting spacecraft. Fabrication process can accurately place dry graphite fibers and overwrap them with aluminum foil, resulting in straight, slender graphite tubes. Graphite fibers pulled out of creeled spools and fed through ceramic eyelets. Spools of aluminum foil mounted on rotating ring and capture graphite fiber as vertical winding machine carriage moves upward. Epoxy resin applied by mechanically spreading epoxy on tetrafluoroethylene mandrel by means of doctor blade attached to carriage.

Bush, H. G.↗

NASA NTRS1998

Probabilistic Modeling of Ceramic Matrix Composite Strength

Uncertainties associated with the primitive random variables such as manufacturing process (processing temperature, fiber volume ratio, void volume ratio), constituent properties (fiber, matrix and interface), and geometric parameters (ply thickness, interphase thickness) have been simulated to quantify the scatter in the first matrix cracking strength (FMCS) and the ultimate tensile strength of SCS-6/RBSN (SiC fiber (SCS-6) reinforced reaction-bonded silicon nitride composite) ceramic matrix composite laminate at room temperature. Cumulative probability distribution function for the FMCS and ultimate tensile strength at room temperature (RT) of (0)(sub 8), (0(sub 2)/90(sub 2), and (+/-45(sub 2))(sub S) laminates have been simulated and the sensitivity of primitive variables to the respective strengths have been quantified. Computationally predicted scatter of the strengths for a uniaxial laminate have been compared with those from limited experimental data. Also the experimental procedure used in the tests has been described briefly. Results show a very good agreement between the computational simulation and the experimental data. Dominating failure modes in (0)(sub 8), (0/90)(sub s) and (+/-45)(sub S) laminates have been identified. Results indicate that the first matrix cracking strength for the (0)(sub S), and (0/90)(sub S) laminates is sensitive to the thermal properties, modulus and strengths of both the fiber and matrix whereas the ultimate tensile strength is sensitive to the fiber strength and the fiber volume ratio. In the case of a (+/-45)(sub S), laminate, both the FMCS and the ultimate tensile strengths have a small scatter range and are sensitive to the fiber tensile strength as well as the fiber volume ratio.

Shan, Ashwin R.↗

NASA NTRS2000

Development of Ceramic Matrix Composite Turbine Blisks for Rocket Engines

Ceramic matrix composite (CMC) integrally bladed turbine disks (blisks) are being considered for use in various advanced propulsion systems for space vehicles. The successful development of this technology can significantly impact National Aeronautics and Space Administration (NASA) space transportation missions, by enabling new efficient systems that can operate at higher temperatures, while reducing costs. Composite blisks comprised of carbon (C) fibers and a silicon carbide (SiC) ceramic matrix were designed, fabricated, characterized, and tested by a multidisciplinary team involving materials, design, structural analysis, turbomachinery, and nondestructive evaluation representatives from government, academia, and industry during a 4.5 year effort led by the NASA Marshall Space Flight Center (MSFC). The testing of several of these blisks, which were developed in the Simplex Turbopump CMC Blisk ]Program for use in rocket engine turbopumps, was recently completed. CMC blisks offer potential advantages in rocket engine turbopumps including increased safety resulting from increased operating temperature margins and greater pump reliability, and decreased costs resulting from improved turbopump performance. The progress that was achieved in that development effort is reviewed, and some of the technology that could be applied to other advanced space transportation propulsion systems is discussed.

Effinger, Mike↗

NASA NTRS2000

Novel Vibration Damping of Ceramic Matrix Composite Turbine Blades Developed for RLV Applications

The Reusable Launch Vehicle (RLV) represents the next generation of space transportation for the U.S. space program. The goal for this vehicle is to lower launch costs by an order of magnitude from $10,000/lb to $1,000/lb. Such a large cost reduction will require a highly efficient operation, which naturally will require highly efficient engines. The RS-2200 Linear Aerospike Engine is being considered as the main powerplant for the RLV. Strong, lightweight, temperature-resistant ceramic matrix composite (CMC) materials such as C/SiC are critical to the development of the RS-2200. Preliminary engine designs subject turbopump components to extremely high frequency dynamic excitation, and ceramic matrix composite materials are typically lightly damped, making them vulnerable to high-cycle fatigue. The combination of low damping and high-frequency excitation creates the need for enhanced damping. Thus, the goal of this project has been to develop well-damped C/SiC turbine components for use in the RLV. Foster-Miller and Boeing Rocketdyne have been using an innovative, low-cost process to develop light, strong, highly damped turbopump components for the RS-2200 under NASA s Small Business Innovation Research (SBIR) program. The NASA Glenn Research Center at Lewis Field is managing this work. The process combines three-dimensionally braided fiber reinforcement with a pre-ceramic polymer. The three-dimensional reinforcement significantly improves the structure over conventional two-dimensional laminates, including high through-the-thickness strength and stiffness. Phase I of the project successfully applied the Foster-Miller pre-ceramic polymer infiltration and pyrolysis (PIP) process to the manufacture of dynamic specimens representative of engine components. An important aspect of the program has been the development of the manufacturing process. Results show that the three-dimensionally braided carbon-fiber reinforcement provides good processability and good mechanical stiffness and strength in comparison to materials produced with competing processes as shown in the graphs.

Min, James B.↗