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NASA NTRS1998

Fabrication Routes for Continuous Fiber-Reinforced Ceramic Composites (CFCC)

The primary approaches used for fabrication of continuous fiber-reinforced ceramic composite (CFCC) components have been reviewed. The CFCC fabrication issues related to fiber, interface, and matrix have been analyzed. The capabilities, advantages and limitations of the five matrix-infiltration routes have been compared and discussed. Today, the best fabrication route for the CFCC end-user is not clear and compromises need to be made depending on the details of the CFCC application. However, with time, this problem should be reduced as research continues to develop advanced CFCC constituents and fabrication routes.

DiCarlo, James A.↗

NASA NTRS1974

Process for fabrication of stabilized aluminum phosphate fibers

Ceramic possesses ideal property combination of high refractoriness and low thermal expansion. Fiber exceeds performance of fused silica fibers at high temperatures. It shrinks less, does not devitrify into unstable cristobalite structure, and is potentially less sensitive to impurities. Might be used for high-temperature insulation, fire protection, composites, and refractories.

Ormiston, T. J.↗

NASA NTRS1995

Affordable Fiber-Reinforced Ceramic Composites Win 1995 R and D 100 Award

Affordable fiber-reinforced ceramic matrix composites (AFReCC) with high strength and toughness, good thermal conductivity, thermal shock resistance, and oxidation resistance are needed for high-temperature structural applications. AFReCC materials will have various applications in advanced high-efficiency and high-performance engines: that is, the High Speed Civil Transport (HSCT), space propulsion components, and land-based systems. For example, silicon-carbide-fiber-reinforced silicon carbide matrix composites show promise for meeting the criteria of high strength, thermal conductivity, and toughness required for the HSCT combustor liner. AFReCC received R&D Magazine's prestigious R&D 100 Award in 1995. The fabrication process for these composites has three steps. In the first step, fiber preforms are made and chemical vapor infiltration is used to apply the desired interface coating on the fibers. This step also rigidizes the preform. The second step consists of resin infiltration, which after pyrolysis, yields an interconnected network of porous carbon as the matrix. In the final step of the process, the carbon-containing preform is infiltrated with molten silicon or silicon alloys in a furnace. This converts the carbon to silicon carbide leaving as little as 5 percent residual free silicon or refractory disilicide phase. This process is suitable for any type of small-diameter fiber (e.g., carbon, alumina, or silicon carbide) woven into a two- or three-dimensional architecture. This processing approach leads to dense composites where matrix microstructure and composition can be tailored for optimum properties. It has much lower processing cost (less than 50 percent) in comparison to other approaches to fabricating silicon-carbide-based composites. The photograph shows the various AFReCC components. Thermomechanical and thermochemical characterization of these composites under the hostile environments that will be encountered in engine applications is underway.

Source record↗

NASA NTRS1986

Ceramic-ceramic shell tile thermal protection system and method thereof

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.

Riccitiello, Salvatore R.↗

NASA NTRS1990

Micromechanical model of crack growth in fiber reinforced ceramics

A model based on the micromechanical mechanism of crack growth resistance in fiber reinforced ceramics is presented. The formulation of the model is based on a small scale geometry of a macrocrack with a bridging zone, the process zone, which governs the resistance mechanism. The effect of high toughness of the fibers in retardation of the crack advance, and the significance of the fiber pullout mechanism on the crack growth resistance, are reflected in this model. The model allows one to address issues such as influence of fiber spacing, fiber flexibility, and fiber matrix friction. Two approaches were used. One represents the fracture initiation and concentrated on the development of the first microcracks between fibers. An exact closed form solution was obtained for this case. The second case deals with the development of an array of microcracks between fibers forming the bridging zone. An implicit exact solution is formed for this case. In both cases, a discrete fiber distribution is incorporated into the solution.

Rubinstein, Asher A.↗

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 NTRS1998

Process for making silicon carbide reinforced silicon carbide composite

A process comprising the steps of: a) providing a fiber preform comprising a non-oxide ceramic fiber with at least one coating, the coating comprising a coating element selected from the group consisting of carbon, nitrogen, aluminum and titanium, and the fiber having a degradation temperature of between 1400.degree. C. and 1450.degree. C., b) impregnating the preform with a slurry comprising silicon carbide particles and between 0.1 wt % and 3 wt % added carbon c) providing a cover mix comprising: i) an alloy comprising a metallic infiltrant and the coating element, and ii) a resin, d) placing the cover mix on at least a portion of the surface of the porous silicon carbide body, e) heating the cover mix to a temperature between 1410.degree. C. and 1450.degree. C. to melt the alloy, and f) infiltrating the fiber preform with the melted alloy for a time period of between 15 minutes and 240 minutes, to produce a ceramic fiber reinforced ceramic composite.

Lau, Sai-Kwing↗

NASA NTRS2001

Silicon carbide reinforced silicon carbide composite

This invention relates to a process comprising the steps of: a) providing a fiber preform comprising a non-oxide ceramic fiber with at least one coating, the coating comprising a coating element selected from the group consisting of carbon, nitrogen, aluminum and titanium, and the fiber having a degradation temperature of between 1400.degree. C. and 1450.degree. C., b) impregnating the preform with a slurry comprising silicon carbide particles and between 0.1 wt % and 3 wt % added carbon c) providing a cover mix comprising: i) an alloy comprising a metallic infiltrant and the coating element, and ii) a resin, d) placing the cover mix on at least a portion of the surface of the porous silicon carbide body, e) heating the cover mix to a temperature between 1410.degree. C. and 1450.degree. C. to melt the alloy, and f) infiltrating the fiber preform with the melted alloy for a time period of between 15 minutes and 240 minutes, to produce a ceramic fiber reinforced ceramic composite.

Lau, Sai-Kwing↗

NASA NTRS1985

Film and interstitial formation of metals in plasma-sprayed ceramics

A method is described to electrodeposit noble metals such as platinum and ordinary metals such as copper on and within plasma-sprayed ceramic materials and ceramic fiber materials. Low-density ceramic fiber bodies were vacuum impregnated with plating solution and attached to an electrode. Light micrographs illustrating the density and location of deposited materials are presented and discussed. Voids in the plasma-sprayed ceramic were filled with deposits that vary from spherical to lens-shaped circular and have particle size corresponding to the full range of void size. Multiple coatings of ceramic and metal can be sequenced.

Hendricks, R. C.↗

NASA NTRS1985

Film and interstitial formation of metals in plasma-sprayed ceramics

Hendricks, R. C.↗

NASA NTRS1995

Low Cost Fabrication of Silicon Carbide Based Ceramics and Fiber Reinforced Composites

A low cost processing technique called reaction forming for the fabrication of near-net and complex shaped components of silicon carbide based ceramics and composites is presented. This process consists of the production of a microporous carbon preform and subsequent infiltration with liquid silicon or silicon-refractory metal alloys. The microporous preforms are made by the pyrolysis of a polymerized resin mixture with very good control of pore volume and pore size thereby yielding materials with tailorable microstructure and composition. Mechanical properties (elastic modulus, flexural strength, and fracture toughness) of reaction-formed silicon carbide ceramics are presented. This processing approach is suitable for various kinds of reinforcements such as whiskers, particulates, fibers (tows, weaves, and filaments), and 3-D architectures. This approach has also been used to fabricate continuous silicon carbide fiber reinforced ceramic composites (CFCC's) with silicon carbide based matrices. Strong and tough composites with tailorable matrix microstructure and composition have been obtained. Microstructure and thermomechanical properties of a silicon carbide (SCS-6) fiber reinforced reaction-formed silicon carbide matrix composites are discussed.

Singh, M.↗

NASA NTRS1991

Effect of fiber reinforcements on thermo-oxidative stability and mechanical properties of polymer matrix composites

A number of studies have investigated the thermo-oxidative behavior of polymer matrix composites. Two significant observations have been made from these research efforts: (1) fiber reinforcement has a significant effect on composite thermal stability; and (2) geometric effects must be considered when evaluating thermal aging data. A compilation of some results from these studies is presented, and this information shows the influence of the reinforcement fibers on the oxidative degradation of various polymer matrix composites. The polyimide PMR-15 was the matrix material that was used in these studies. The control composite material was reinforced with Celion 6000 graphite fiber. T-40R graphite fibers, along with some very stable ceramic fibers were selected as reinforcing fibers because of their high thermal stability. The ceramic fibers were Nicalon (silicon carbide) and Nextel 312 (alumina-silica-boron oxide). The mechanical properties of the two graphite fiber composites were significantly different, probably owing to variations in interfacial bonding between the fibers and the polyimide matrix. The Celion 6000/PMR-15 bond is very tight but the T-40/PMR-15 bond is less tight. Three oxidation mechanisms were observed: (1) the preferential oxidation of the Celion 6000 fiber ends at cut surfaces, leaving a surface of matrix material with holes where the fiber ends were originally situated; (2) preferential oxidation of the composite matrix; and (3) interfacial degradation by oxidation. The latter two mechanisms were also observed on fiber end cut surfaces. The fiber and interface attacks appeared to initiate interfiber cracking along these surfaces.

Bowles, Kenneth J.↗

NASA NTRS1992

Effect of fiber reinforcement on thermo-oxidative stability and mechanical properties of polymer matrix composites

A number of studies have investigated the thermooxidative behavior of polymer matrix composites. Two significant observations have been made from these research efforts: (1) fiber reinforcement has a significant effect on composite thermal stability; and (2) geometric effects must be considered when evaluating thermal aging data. The polyimide PMR-15 was the matrix material used in these studies. The control composite material was reinforced with Celion 6000 graphite fiber. T-4OR graphite fibers, along with some very stable ceramic fibers were selected as reinforcing fibers because of their high thermal stability. The ceramic fibers were Nicalon (silicon carbide) and Nextel 312 (alumina-silica-boron oxide). The mechanical properties of the two graphite fiber composites were significantly different, probably owing to variations in interfacial bonding between the fibers and the polyimide matrix. Three oxidation mechanisms were observed: (1) the preferential oxidation of the Celion 6000 fiber ends at cut surfaces, leaving a surface of matrix material with holes where the fiber ends were originally situated; (2) preferential oxidation of the composite matrix; and (3) interfacial degradation by oxidation. The latter two mechanisms were also observed on fiber end cut surfaces. The fiber and interface attacks appeared to initiate interfiber cracking along these surfaces.

Bowles, K. J.↗

NASA NTRS1995

Bend stress relaxation and tensile primary creep of a polycrystalline alpha-SiC fiber

Understanding the thermomechanical behavior (creep and stress relaxation) of ceramic fibers is of both practical and basic interest. On the practical level, ceramic fibers are the reinforcement for ceramic matrix composites which are being developed for use in high temperature applications. It is important to understand and model the total creep of fibers at low strain levels where creep is predominantly in the primary stage. In addition, there are many applications where the component will only be subjected to thermal strains. Therefore, the stress relaxation of composite consituents in such circumstances will be an important factor in composite design and performance. The objective of this paper is to compare and analyze bend stress relaxation and tensile creep data for alpha-SiC fibers produced by the Carborundum Co. (Niagara Falls, NY). This fiber is of current technical interest and is similar in composition to bulk alpha-SiC which has been studied under compressive creep conditions. The temperature, time, and stress dependences will be discussed for the stress relaxation and creep results. In addition, some creep and relaxation recovery experiments were performed in order to understand the complete viscoelastic behavior, i.e. both recoverable and nonrecoverable creep components of these materials. The data will be presented in order to model the deformation behavior and compare relaxation and/or creep behavior for relatively low deformation strain conditions of practical concern. Where applicable, the tensile creep results will be compared to bend stress relaxation data.

Hee Man, Yun↗

NASA NTRS1997

Method to Produce Flexible Ceramic Thermal Protection System Resistant to High Aeroacoustic Noise

A method of producing a three dimensional angle interlock ceramic fiber which is stable to high aeroacoustic noise of about 170 decibels and to high temperatures of about 2500 F is disclosed. The method uses multiple separate strands of a ceramic fiber or ceramic tow suitable for weaving having multiple warp fibers and multiple fill fibers woven with a modified fly-shuttle loom or rapier shuttleless loom which has nip rolls, a modified fabric advancement mechanism and at least eight harnesses in connection with a Dobby pattern chain utilizing sufficient heddles for each warp fiber and a reed which accommodates at least 168 ends per inch. The method produces a multilayered top fabric, rib fabric and single-layered bottom fabric.

Sawko, Paul M.↗

NASA NTRS1990

Production of continuous mullite fiber via sol-gel processing

The development of a continuous ceramic fiber which could be used in rocket engine and rocket boosters applications was investigated at the Marshall Space Flight Center. Methods of ceramic fiber production such as melt spinning, chemical vapor deposition, and precursor polymeric fiber decomposition are discussed and compared with sol-gel processing. The production of ceramics via the sol-gel method consists of two steps, hydrolysis and polycondensation, to form the preceramic, followed by consolidation into the glass or ceramic structure. The advantages of the sol-gel method include better homogeneity and purity, lower preparation temperature, and the ability to form unique compositions. The disadvantages are the high cost of raw materials, large shrinkage during drying and firing which can lead to cracks, and long processing times. Preparation procedures for aluminosilicate sol-gel and for continuous mullite fibers are described.

Tucker, Dennis S.↗

NASA NTRS1991

Ultrasonic velocity technique for monitoring property changes in fiber-reinforced ceramic matrix composites

A technique for measuring ultrasonic velocity was used to monitor changes that occur during processing and heat treatment of a SiC/RBSM composite. Results indicated that correlations exist between the ultrasonic velocity data and elastic modulus and interfacial shear strength data determined from mechanical tests. The ultrasonic velocity data can differentiate strength. The advantages and potential of this nondestructive evaluation method for fiber reinforced ceramic matrix composite applications are discussed.

Kautz, Harold E.↗

NASA NTRS1991

Ultrasonic velocity technique for monitoring property changes in fiber-reinforced ceramic matrix composites

A technique for measuring ultrasonic velocity was used to monitor changes that occur during processing and heat treatment of a SiC/RBSM composite. Results indicated that correlations exist between the ultrasonic velocity data and elastic modulus and interfacial shear strength data determined from mechanical tests. The ultrasonic velocity data can differentiate strength. The advantages and potential of this nondestructive evaluation method for fiber reinfoced ceramic matrix composite applications are discussed.

Kautz, H. E.↗