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All sourcesNASA NTRSDOE OSTI
NASA NTRS2017

Environmental Barrier Coatings for Ceramic Matrix Composites - An Overview

SiC/SiC Ceramic Matrix Composites (CMCs) are increasingly being considered as structural materials for advanced power generation equipment because of their light weight, higher temperature capability, and oxidation resistance. Limitations of SiC/SiC CMCs include surface recession and component cracking and associated chemical changes in the CMC. The solutions pursued to improve the life of SiC/SiC CMCs include the incorporation of coating systems that provide surface protection, which has become known as an Environmental Barrier Coating (EBC). The development of EBCs for the protection of gas turbine hot section CMC components was a continuation of coating development work for corrosion protection of silicon-based monolithics. Work on EBC development for SiC/SiC CMCs has been ongoing at several national laboratories and the original gas turbine equipment manufacturers. The work includes extensive laboratory, rig and engine testing, including testing of EBC coated SiC/SiC CMCs in actual field applications. Another EBC degradation issue which is especially critical for CMC components used in aircraft engines is the degradation from glassy deposits of calcium-magnesium-aluminosilicate (CMAS) with other minor oxides. This paper addresses the need for and properties of external coatings on SiC/SiC CMCs to extend their useful life in service and the retention of their properties.

EBC↗
DOE OSTI2026

Review of SiC material development for nuclear fusion applications: Cross-cutting research and emerging opportunities

The SiC-based materials, particularly SiC-fiber-reinforced SiC matrix (SiC/SiC) composites, show strong potential for structural and functional applications in future fusion power plants because they can operate at high temperatures with a range of coolants and breeders, thereby enabling higher energy conversion efficiency. Here, this paper presents recent advancements in the development of SiC-based materials, focusing on processing techniques and material performance and resistance under fusion-relevant environments. The processing activities have emphasized near-net-shape fabrication and the joining of SiC subcomponents, with processing methods and material compositions informed by previous irradiation experiments on various grades of SiC. Research on irradiation effects has remained focused on degradation mechanisms and the microstructural optimization of SiC/SiC composites irradiated to high neutron damage levels. Analysis of irradiation defects in SiC has advanced via the application of cutting-edge characterization methods, among which Raman spectroscopy is becoming a common tool to assess atomic-scale chemical disorder. Fusion–fission crosscutting irradiation research has explored combined effects in SiC/SiC composites with application-relevant geometries, including bowing of SiC/SiC composite channels under neutron flux gradients, stress evolution in SiC/SiC composite tubes under through-thickness temperature gradients, and irradiation-enhanced corrosion in SiC. Finally, research opportunities for component testing and assessment under fusion-relevant conditions, in support of emerging concepts from the private fusion sector, are discussed.

Advanced manufacturing↗
DOE OSTI2022

Mach Conference, 2022.

There has been considerable interest in chemical vapor infiltration (CVI) manufactured silicon carbide fiber and silicon carbide matrix (SiC/SiC) composite tubes due to their superior mechanical properties. The SiC/SiC tubes are known to remain stable even after prolonged exposure to radiation. However, there are many variables in the manufacturing of SiC/SiC composite tubes such as elastic constants of constituent SiC fiber and SiC matrix, braiding angle, porosity, and others whose values vary over a range. The intention is to identify the distribution of elastic constants of SiC/SiC tubes which would help model the performance of the novel cladding material. To do so, a sensitivity analysis will be carried out to determine the dominant variables that influence the elastic constants of SiC/SiC tubes. A chosen number of combinations of dominant variables will be sampled through the Latin hypercube sampling (LHS) method. The elastic constants of composite tube namely Young's moduli in the circumferential and longitudinal direction, Poisson's ratio, and shear modulus will be calculated at sampled points through finite element (FE) analysis. A polynomial response surface (PRS) will be built for each of the elastic constants to be used as a surrogate to FE analysis. Once the predictive accuracy of PRS is verified at the validation set of data points, the PRS will be invoked 105 times in Monte Carlo simulations (MCS). The uncertainty can be quantified by calculating the coefficient of variation (CV) based on MCS-generated data which will be presented at the conference.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
NASA NTRS2005

Factors Controlling Elevated Temperature Strength Degradation of Silicon Carbide Composites

For 5 years, the cooperative agreement NCC3-763 has focused on the development and understanding of Sic-based composites. Most of the work was performed in the area of SiC fiber-reinforced composites for UEET and NGLT and in collaboration with Goodrich Corporation under a partially reimbursable Space Act Agreement. A smaller amount of work was performed on C fiber-reinforced SiC matrix composites for NGLT. Major accomplishments during this agreement included: Improvements to the interphase used in melt-infiltrated (MI) SiC/SiC composites which increases the life under stressed-oxidation at intermediate temperatures referred to as "outside-debonding". This concept is currently in the patent process and received a Space Act Award. Mechanistic-based models of intermediate temperature degradation for MI SiC/SiC Quantification and relatively robust relationships for matrix crack evolution under stress in SiC/SiC composites which serve as the basis for stress-strain and elevated temperature life models The furthering of acoustic emission as a useful tool in composite damage evolution and the extension of the technique to other composite systems Development of hybrid C-SiC fiber-reinforced SiC matrix composites Numerous presentations at conferences, industry partners, and government centers and publications in recognized proceedings and journals. Other recognition of the author's accomplishments by NASA with a TGIR award (2004), NASA's Medal for Public Service (2004), and The American Ceramic Society s Richard M. Fulrath Award (2005). The following will briefly describe the work of the past five years in the three areas of interest: SiC/SiC composite development, mechanistic understanding and modeling of SiC/SiC composites, and environmental durability of C/SiC composites. More detail can be found in the publications cited at the end of this report.

Source record↗
NASA NTRS2002

Architectures for High-Performance Ceramic Composites Being Improved

A major thrust of the Ultra-Efficient Engine Technology (UEET) Program at the NASA Glenn Research Center is to develop advanced hot-section engine components using SiC/SiC ceramic matrix composites (CMC's) with thermostructural capability to 2400 F (1315 C). In previous studies, UEET determined that the higher the ultimate tensile strength (UTS) of the as-fabricated CMC, the greater its structural performance at 2400 F. Thus efforts have been ongoing within UEET to understand and develop fiber architecture approaches that can improve the UTS of SiC/SiC CMC's. Under UEET, SiC/SiC test panels and demonstration engine components are currently produced by the multi-ply layup of two-dimensional fabric pieces. The fabric is typically formed of multifilament tows containing high-performance Sylramic (Dow Corning) SiC fiber that is woven into two-dimensional five-harness satin fabric with 20 ends per inch in the 0 degree and 90 degree directions. In some cases, fabric pieces containing woven Sylramic fiber tows are thermally treated at NASA to form Sylramic-iBN fibers that contain a very thin in-situ-grown boron nitride layer on their surfaces. The final SiC/SiC panels and components are fabricated at the CMC vendor by compressing the fabric pieces in tools and then depositing a thin BN interphase coating on the fibers by chemical vapor deposition. The last step at the vendor is to infiltrate the BN-coated fiber architecture with SiC and silicon matrix constituents to form a dense product. Because the as-produced Sylramic fiber tows are sized with a thin polymer coating to facilitate handling and weaving, the individual fibers within the tows and fabric are in close contact with each other. This contact is further increased during fabric compression. One important recent finding is that increasing Sylramic fiber tow width in a fabric increases the UTS of the final SiC/SiC CMC. This effect is presumably related to minimizing fiber/fiber contact, which can be detrimental to CMC strength because of the boron-rich chemistry and roughness of the Sylramic fiber surface. Tows can be spread by mechanically agitating the Sylramic fabric prior to CMC fabrication or by simply thermally treating the Sylramic fabric as in the formation of the Sylramic-iBN fibers. However, CMC's with the treated Sylramic-iBN fabric are even stronger than CMC's with mechanically spread Sylramic tows. The extra strength capability is presumably related to the in situ BN on the fiber surface, which adds compliance to the fiber surfaces and is more resistant to oxygen impurities introduced during the chemical vapor deposition BN process. As shown, another important finding is that the use of fabric with tows having less than the standard of 20 ends per inch provides advantages in terms of reduced ply height and increased ply and CMC strength. The reduced ply height provides more control of part thickness by allowing more plies for a given thickness and by reducing interlaminar residual stresses between plies. The increased ply strength is presumably related to a reduced number of interlaced 90 tows, which, in turn, reduces the crimp angle on the high-modulus fibers in the 0 degree tows. Also, as shown, although fabric with fewer ends per inch reduced the maximum fiber fraction in an eight-ply CMC panel; CMC UTS actually increased because of increased ply strength. Thus, using fabric with fewer ends per inch has several advantages, including providing a significantly higher strength per fiber fraction in the CMC. Consequently, ongoing UEET efforts will attempt to use architectural approaches for components that minimize fiber-fiber contacts and fiber bending within the final composite microstructure.

Yun, Hee Mann↗
DOE OSTI2021

HFIR SiC Bowing Test Ready to Insert

This report describes the successful assembly of a High Flux Isotope Reactor (HFIR) irradiation experiment designed to assess radiation-induced lateral bowing of silicon carbide fiber–reinforced, silicon carbide matrix composite (SiC/SiC) components under a radial fast neutron flux gradient. Excessive bowing of a SiC/SiC channel box in a boiling water reactor could potentially interfere with control blade movements. Similar concerns exist for SiC/SiC fuel cladding in light water reactors. The experiment described herein will provide experimental validation of the structural response of a miniature SiC/SiC channel box and tube specimens with pressurized water reactor diameters during irradiation. The significant radial fast neutron flux gradients that exist in the permanent reflector of HFIR were characterized using detailed three-dimensional neutronic calculations. The three-dimensional displacement damage dose rate profile and the resulting volumetric swelling in SiC were used as inputs to structural analyses that predicted the deformation and stresses in the channel box specimen. The specimens were thoroughly characterized prior to irradiation using traditional dimensional inspection and surface profilometry so that these measurements can later be compared with similar measurements that will be made post-irradiation to determine radiation-induced deformations. Furthermore, fine engraving markers were inscribed along all outer surfaces of the specimen and mapped using a digital microscope and a three-dimensional stage. This technique allowed for accurate measurements of the marker spacings, which can be compared with similar measurements that will be made post-irradiation to provide local radiation-induced strain mapping. The experiment was successfully assembled and is scheduled for insertion during HFIR cycle 492, which is currently scheduled to run from May 25, 2021 to June 18, 2021.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2025

Conceptual Designs for Irradiation Creep Testing of SiC in HFIR

Understanding irradiation creep of nuclear fuel cladding is important to properly size the initial fuel-cladding gap and understand when pellet-cladding contact is expected to occur due to a combination of fuel swelling and cladding creep-down. Irradiation creep also plays a role in relaxing stresses that develop in-pile. Silicon carbide fiber–reinforced silicon carbide matrix (SiC/SiC) composites are the leading long-term accident-tolerant fuel cladding concept for light-water reactors (LWRs). Although some limited data are available regarding irradiation creep of the individual constituents (fibers, matrix), data regarding irradiation creep of SiC/SiC composites are currently insufficient. Additional data regarding irradiation creep compliance and the rupture lifetime (combination of creep and slow crack growth) are needed to understand material limitations. This work describes the design and development of two irradiation vehicles that are being pursued for testing SiC/SiC concepts in the High Flux Isotope Reactor (HFIR). The first is a passive experiment, referred to as the PRECISE experiment, that leverages the constant coolant pressure of HFIR to compress a metallic bellows and provide a well-characterized load to drive creep in a SiC/SiC dog bone specimen. The total creep strain would be quantified post-irradiation by measuring dimensional changes of the specimen length as well as local dimensional changes within the gauge region. Non-stressed specimens would also be irradiated under the same conditions to provide an indication of dimensional changes due to radiation-induced swelling in the absence of creep. A second, more complex experiment, referred to as the INSITE experiment, is being designed in parallel that would use pneumatics to pressurize a metal bellows and linear variable differential transformers (LVDTs) to measure the specimen displacement in situ during irradiation. Such an experiment would provide significantly more data regarding the evolution of the creep compliance as a function of dose and applied stress within a single experiment but would require significantly more development time and cost to execute. The primary concern with the INSITE experiment is the accuracy, reliability, and expected lifetime of the LVDTs during irradiation at elevated temperatures. Efforts are being made to adjust the experiment design and operating procedure to limit LVDT temperatures and mitigate or otherwise compensate for uncertainties due to factors such as temperature fluctuations, creep in the surrounding structural materials, and drift of the LVDTs. This work describes the experiment designs, thermal and structural analysis that were performed to ensure that the desired temperature and stress conditions can be achieved, some initial sensitivity analyses to predict the evolution of the radiation-induced specimen displacements, and potential sources of uncertainty in the measurements. Out-of-pile testing is being performed in parallel to confirm that the test trains achieve the expected stress states in the specimens and do not result in prohibitive stress concentrators (e.g., in the grip regions) that might risk pre-mature failure. The PRECISE experiments are proceeding toward fabrication and assembly with HFIR insertion planned during fiscal year 2026. The INSITE experiment is progressing toward out-of-pile demonstrations, which will provide more conclusive evidence regarding the feasibility of executing these tests in HFIR or whether alternative displacement monitoring techniques may need to be considered.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1999

Sensor Lead Wires Positioned on SiC-based Monolithic Ceramic and Fiber- reinforced Ceramic Matrix Composite Subcomponents with Flat and Curved Surfaces

There is strong interest in the development of silicon carbide-based monolithic ceramic and composite materials and components for demanding, high-temperature applications. Thorough characterization of material properties, including high-temperature testing under simulated or actual operating conditions, is a high priority for programs involved in developing these silicon carbide- (SiC) based materials and components. Members of the Sensors and Electronics Technology Branch at the NASA Lewis Research Center are developing minimally intrusive methods of measuring the properties (such as the surface temperature, strain, and heat flux characteristics) of components and subelements that are being tested or operated in hostile, high-temperature environments. Their primary goal is to instrument the test article or operating component with durable sensors that have a minimal effect on test conditions such as the gas flow across the surface of the item and the material response (including the through-thickness conduction of heat). Therefore, the main thrust of their work has been the development of thin-film sensors (e.g., thermocouples or strain gauges) for use on various advanced material test articles, including SiC/SiC composite components. There was a need for a better method of securing sensor lead wires on SiC-based components and subelements that would be tested at temperatures to 1000 C (or higher), to enhance the durability of the overall minimally intrusive sensor system. To address this need, Lewis researchers devised an alternative approach for positioning the sensor lead wires (which are connected to the thin-film sensors) on SiC or SiC/SiC components. A reaction-forming method of joining was used to strongly bond hoop-shaped monolithic SiC and SiC/SiC composite attachments of various sizes to both flat and curved surfaces of SiC/SiC composite subelements (see the photos). This approach is based on an affordable, robust ceramic joining technology, named ARCJoinT, which was developed at Lewis for the joining of SiC-based ceramics and fiber-reinforced composites.

Kiser, James D.↗
DOE OSTI2020

Microstructure Experiments-Enabled MARMOT Simulations of SiC/SiC-based Accident Tolerant Nuclear Fuel System

We have undertaken an experimental-computational project that addresses a few key technology gaps associated with the use of SiC/SiC composites for light water reactor fuel cladding. Two principal endeavors in this project are to assess the irradiation-induced microstructural changes and swelling in SiC/SiC composites, and to characterize and model the porous oxide surface layer (when exposed to steam) along SiC recession that is detrimental to the clad integrity under accident conditions. The project tasks are: (i) ion irradiation and characterization (University of Tennessee, Knoxville), (ii) mechanical tests and analysis (University of South Carolina), (iii) steam exposure tests (Oak Ridge National Laboratory), (iv) electron microscopy and spectroscopic characterization (NC State University), (v) x-ray microscopy and reconstruction (University of South Carolina and NC State University), (vi) phase field modeling and simulations (NC State University and Idaho National Laboratory). The effects of 10 MeV Au ion irradiation at 350°C on the microstructure evolution in SiC/SiC composites are investigated at doses up to 400 displacements per atom (dpa) at the University of Tennessee, Knoxville. Atomic force microscopy and optical profilometry reveal irradiation induced axial and radial shrinkage of the fibers for doses greater than 10 dpa. Based on detailed electron microscopy characterization, the primary cause of the fiber shrinkage is attributed to irradiation-induced loss of carbon packets. Additionally, the multilayer PyC interface is observed to portray high resistance to irradiation damage. The mechanical response and failure mechanisms of un-irradiated samples is also assessed through loading tests and X-ray imaging at the University of South Carolina. Steam exposure tests are performed at the Oak Ridge National Laboratory in a facility that represents a reactor pressure vessel under a loss-of-coolant-accident scenario. The samples that are analyzed methodically in this report are tested for 32/31 hours at 1200°C with a velocity of 0.25 cm/s for the pressures: 0.1 MPa, 0.45 MPa, 0.92 MPa and 1.38 MPa. Scanning/transmission electron microscopy analysis conducted at the NC State University (NCSU) shows that the oxide layer thickness increases with the steam pressure. While the oxide layer is crystalline (α- cristobalite) for the pressures 0.45 MPa, 0.92 MPa and 1.38 MPa, the layer is amorphous at 0.1 MPa. Results from Raman spectroscopy have also confirmed the formation of α-cristobalite phase of SiO₂. The abrupt increase in the integrated Raman intensity ratio between steam pressures 0.1 and 0.45 MPa suggests the onset of accelerated crystallization. Non-destructive three dimensional X-ray microscopy/tomography (XCT) and computational image processing techniques are employed by the University of South Carolina to probe the porous oxidation features on SiC samples at varying pressures. Interestingly, most pores are observed to be located away from the surface as well as the oxide-SiC interface. The average oxide layer thickness assessed from the XCT analysis is seen to be in excellent agreement with the values determined through scanning electron microscopy analysis for the highest pressures where the oxide layer is relatively more uniform. A phase-field model developed by the NC State University and Idaho National Laboratory for simulating oxidation of SiC by steam captures the paralinear kinetics of SiC oxidation with a high degree of fidelity. Results from quasi-one-dimensional and two dimensional simulations show that the pores with oxidizing species lead to a higher volatilization rate. These simulations indicate that the enhanced apparent volatilization rates at higher pressures observed in experiments can be rationalized by the increased volatilization from the pores. The project team has also successfully developed the capability to import images from experiments for realistic evolution of the oxidizing microstructure.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

The response of accident tolerant fuel cladding to LOCA burst testing: A comparative study of leading concepts

Accident tolerant fuel claddings seek to improve safety margins during loss-of-coolant accident (LOCA) scenarios by reducing cladding steam oxidation rates, hydrogen production, delaying or mitigating cladding burst, and reducing cladding deformation. After rapid and extensive progress in recent years, Cr coated Zr-based alloys, ferritic FeCrAl, and SiC/SiC ceramic matrix composites (CMCs) have emerged as the most promising cladding concepts, but there are few studies comparing the accident tolerance of all three concepts simultaneously. Here, in this study, LOCA burst testing has been conducted on Cr high impulse power magnetron sputtered Zry-4 (Cr/Zry-4), C26M (FeCrAl), and SiC/SiC SiGA (CMC). Experimental observations indicate Cr/Zry-4 burst at higher temperatures than Zry-4 however the effectiveness of the coating on mitigating ZrO 2 formation via Cr 2 O 3 formation depended on physical proximity to the burst opening. No dramatic improvement in diametrical strain nor opening geometry was observed. C26M burst at higher temperatures than Zry-4 at lower pressures, exhibiting small amounts of strain and smaller openings, and formed slow-growing Al 2 O 3 regardless of location. The CMCs did not burst or show any macroscopic signs of deformation, all the way up to an internal cladding pressure of 15.2 MPa. High temperature expanding Nb plug testing indicated that CMC room temperature strength may persist up to 1650°C, with an approximately 40% loss of strength at 1900°C. CMC steam oxidation was also compared to reference chemically vapor deposited SiC up to 1700°C, and CMCs were found to oxidize at slightly accelerated rates that were still orders of magnitude lower than bare Zry-4. Projected H 2 generation during LOCA burst testing showed that when accounting for cladding burst exposing inner diameters to steam, Cr coated Zry-4 reduced H 2 generation by a factor of two compared with bare Zry-4, while both C26M and SiC/SiC reduced H 2 generation by orders of magnitude relative to bare Zry-4.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Integrated TBC/EBC for SiC Fiber Reinforced SiC Matrix Composites for Next Generation Gas Turbines (Final Report)

In this ambitious project, a significant challenge preventing widespread use of ceramic matrix composites in hot section components of gas power generating turbines was addressed. Hot section components made from SiC fiber reinforced SiC matrix composites (SiC/SiC composites), have the potential to achieve a combined cycle energy efficiency of above 65%. To achieve this efficiency, the temperature of the combustion gases on the turbine component surface is expected to reach as high as ~1700ºC (3100ºF). However, SiC/SiC composites suffer from volatilization at high temperature under high velocity steam environment – typical in a turbine hot chamber. This integrated collaborative project, between two research groups at Clemson University and a team of engineers and scientists at GE Gas Power, focused on design, fabrication and evaluation of a new graded environmental barrier coating. Using the excellent compositional tailorability of polymer derived ceramics (PDCs), we developed an integrated EBC/BC that smoothly transitions from bottom SiC/SiC bond interface to hermetic sesquioxide (Y 2 O 3 ) top surface. This smooth compositional transition avoided the sharp CTE mismatch at interfaces to greatly reduce the thermal stress. The developed EBC is compatible with and bonds well with the bond coat that GE uses. The top hermetic oxide surface ensures low oxygen transportation and volatilization rates under the high velocity steam environment. The graded microstructure with increasing sesquioxide concentration also decreases the amount of Si and C elements near the top hermetic sesquioxide layer. Coatings made using a process suitable for manufacturing – atmospheric plasma spraying was demonstrated. The microstructure of coatings made using this process were fully characterized. Finally, the performance of these coatings was investigated under the most demanding conditions for this application. Specifically, high temperature, high velocity steam exposure; thermal shock test; and thermal cycling tests. The graded coatings performed exceptionally well in all these tests. Specific suggestions for future development in this area have also been identified. In addition to the excellent technical progress, this project helped initiate a robust collaboration between the research groups at Clemson and GE Gas Power. It also provided a high-quality learning and mentoring opportunity for the three post-doctoral research associates and two UG students at Clemson University who worked on this project. All proposed tasks, sub-tasks were completed, and all milestones achieved.

03 NATURAL GAS↗
NASA NTRS2000

Turbine Airfoil With CMC Leading-Edge Concept Tested Under Simulated Gas Turbine Conditions

Silicon-based ceramics have been proposed as component materials for gas turbine engine hot-sections. When the Navy s Harrier fighter experienced engine (Pegasus F402) failure because of leading-edge durability problems on the second-stage high-pressure turbine vane, the Office of Naval Research came to the NASA Glenn Research Center at Lewis Field for test support in evaluating a concept for eliminating the vane-edge degradation. The High Pressure Burner Rig (HPBR) was selected for testing since it could provide temperature, pressure, velocity, and combustion gas compositions that closely simulate the engine environment. The study focused on equipping the stationary metal airfoil (Pegasus F402) with a ceramic matrix composite (CMC) leading-edge insert and evaluating the feasibility and benefits of such a configuration. The test exposed the component, with and without the CMC insert, to the harsh engine environment in an unloaded condition, with cooling to provide temperature relief to the metal blade underneath. The insert was made using an AlliedSignal Composites, Inc., enhanced HiNicalon (Nippon Carbon Co. LTD., Yokohama, Japan) fiber-reinforced silicon carbide composite (SiC/SiC CMC) material fabricated via chemical vapor infiltration. This insert was 45-mils thick and occupied a recessed area in the leading edge and shroud of the vane. It was designed to be free floating with an end cap design. The HPBR tests provided a comparative evaluation of the temperature response and leading-edge durability and included cycling the airfoils between simulated idle, lift, and cruise flight conditions. In addition, the airfoils were aircooled, uniquely instrumented, and exposed to the exact set of internal and external conditions, which included gas temperatures in excess of 1370 C (2500 F). In addition to documenting the temperature response of the metal vane for comparison with the CMC, a demonstration of improved leading-edge durability was a primary goal. First, the metal vane was tested for a total of 150 cycles. Both the leading edge and trailing edge of the blade exhibited fatigue cracking and burn-through similar to the failures experienced in service by the F402 engine. Next, an airfoil, fitted with the ceramic leading edge insert, was exposed for 200 cycles. The temperature response of those HPBR cycles indicated a reduced internal metal temperature, by as much as 600 F at the midspan location for the same surface temperature (2100 F). After testing, the composite insert appeared intact, with no signs of failure on either the vane s leading or trailing edge. Only a slight oxide scale, as would be expected, was noted on the insert. Overall, the CMC insert performed similarly to a thick thermal barrier coating. With a small air gap between the metal and the SiC/SiC leading edge, heat transfer from the CMC to the metal alloy was low, effectively lowering the temperatures. The insert's performance has proven that an uncooled CMC can be engineered and designed to withstand the thermal up-shock experienced during the severe lift conditions in the Pegasus engine. The design of the leading-edge insert, which minimized thermal stresses in the SiC/SiC CMC, showed that the CMC/metal assembly can be engineered to be a functioning component.

Robinson, R. Craig↗
NASA NTRS2002

New High-Performance SiC Fiber Developed for Ceramic Composites

Sylramic-iBN fiber is a new type of small-diameter (10-mm) SiC fiber that was developed at the NASA Glenn Research Center and was recently given an R&D 100 Award for 2001. It is produced by subjecting commercially available Sylramic (Dow Corning, Midland, MI) SiC fibers, fabrics, or preforms to a specially designed high-temperature treatment in a controlled nitrogen environment for a specific time. It can be used in a variety of applications, but it currently has the greatest advantage as a reinforcement for SiC/SiC ceramic composites that are targeted for long-term structural applications at temperatures higher than the capability of metallic superalloys. The commercial Sylramic SiC fiber, which is the precursor for the Sylramic-iBN fiber, is produced by Dow Corning, Midland, Michigan. It is derived from polymers at low temperatures and then pyrolyzed and sintered at high temperatures using boron-containing sintering aids (ref. 1). The sintering process results in very strong fibers (>3 GPa) that are dense, oxygen-free, and nearly stoichiometric. They also display an optimum grain size that is beneficial for high tensile strength, good creep resistance, and good thermal conductivity (ref. 2). The NASA-developed treatment allows the excess boron in the bulk to diffuse to the fiber surface where it reacts with nitrogen to form an in situ boron nitride (BN) coating on the fiber surface (thus the product name of Sylramic-iBN fiber). The removal of boron from the fiber bulk allows the retention of high tensile strength while significantly improving creep resistance and electrical conductivity, and probably thermal conductivity since the grains are slightly larger and the grain boundaries cleaner (ref. 2). Also, as shown in the graph, these improvements allow the fiber to display the best rupture strength at high temperatures in air for any available SiC fiber. In addition, for CMC applications under oxidizing conditions, the formation of an in situ BN surface layer creates a more environmentally durable fiber surface not only because a more oxidation-resistant BN is formed, but also because this layer provides a physical barrier between contacting fibers with oxidation-prone SiC surface layers (refs. 3 and 4). This year, Glenn demonstrated that the in situ BN treatment can be applied simply to Sylramic fibers located within continuous multifiber tows, within woven fabric pieces, or even assembled into complex product shapes (preforms). SiC/SiC ceramic composite panels have been fabricated from Sylramic-iBN fabric and then tested at Glenn within the Ultra-Efficient Engine Technology Program. The test conditions were selected to simulate those experienced by hot-section components in advanced gas turbine engines. The results from testing at Glenn demonstrate all the benefits expected for the Sylramic-iBN fibers. That is, the composites displayed the best thermostructural performance in comparison to composites reinforced by Sylramic fibers and by all other currently available high-performance SiC fiber types (refs. 3 and 5). For these reasons, the Ultra-Efficient Engine Technology Program has selected the Sylramic-iBN fiber for ongoing efforts aimed at SiC/SiC engine component development.

DiCarlo, James A.↗
NASA NTRS2004

Advanced Constituents and Processes for Ceramic Composite Engine Components

The successful replacement of metal alloys by ceramic matrix composites (CMC) in hot-section engine components will depend strongly on optimizing the processes and properties of the CMC microstructural constituents so that they can synergistically provide the total CMC system with improved temperature capability and with the key properties required by the components for long-term structural service. This presentation provides the results of recent activities at NASA aimed at developing advanced silicon carbide (Sic) fiber-reinforced hybrid Sic matrix composite systems that can operate under mechanical loading and oxidizing conditions for hundreds of hours at 2400 and 2600 F, temperatures well above current metal capability. These SiC/SiC composite systems are lightweight (-30% metal density) and, in comparison to monolithic ceramics and carbon fiber-reinforced ceramic composites, are able to reliably retain their structural properties for long times under aggressive engine environments. It is shown that the improved temperature capability of the SiC/SiC systems is related first to the NASA development of the Sylramic-iBN Sic fiber, which displays high thermal stability, creep resistance, rupture resistance, and thermal conductivity, and possesses an in-situ grown BN surface layer for added environmental durability. This fiber is simply derived from Sylramic Sic fiber type that is currently produced at ATK COI Ceramics. Further capability is then derived by using chemical vapor infiltration (CVI) to form the initial portion of the hybrid Sic matrix. Because of its high creep resistance and thermal conductivity, the CVI Sic matrix is a required base constituent for all the high temperature SiC/SiC systems. By subsequently thermo- mechanical-treating the CMC preform, which consists of the S ylramic-iBN fibers and CVI Sic matrix, process-related defects in the matrix are removed, further improving matrix and CMC creep resistance and conductivity.

Yun, H. M.↗
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 NTRS2012

An Update on Design Tools for Optimization of CMC 3D Fiber Architectures

Objective: Describe and up-date progress for NASA's efforts to develop 3D architectural design tools for CMC in general and for SIC/SiC composites in particular. Describe past and current sequential work efforts aimed at: Understanding key fiber and tow physical characteristics in conventional 2D and 3D woven architectures as revealed by microstructures in the literature. Developing an Excel program for down-selecting and predicting key geometric properties and resulting key fiber-controlled properties for various conventional 3D architectures. Developing a software tool for accurately visualizing all the key geometric details of conventional 3D architectures. Validating tools by visualizing and predicting the Internal geometry and key mechanical properties of a NASA SIC/SIC panel with a 3D orthogonal architecture. Applying the predictive and visualization tools toward advanced 3D orthogonal SiC/SIC composites, and combining them into a user-friendly software program.

Lang, J.↗
NASA NTRS2019

Characterizing Early Damage Evolution in CMCs

Silicon carbide / silicon carbide ceramic matrix composites (SiC/SiC CMCs) are structural ceramics that are well-suited for the extreme environment conditions of space and aerospace applications largely due to their low weight, creep resistance, damage tolerance, and high specific strength. In CMCs, the initiation and accumulation of damage depends on characteristics of the constituent landscape including porosity, interfacial properties, and geometric distribution of CMC constituents. In order to accurately predict the lifetimes of these advanced composites, it is critical to understand the evolution of damage and to characterize which early damage mechanisms subsequently lead to crack coalescence and macroscopic failure. In this study, SiC/SiC minicomposites are characterized through an experimental approach combining acoustic emission (AE) with tensile testing in-SEM (scanning electron microscope), in order to examine early damage initiation (below the proportional limit) and its evolution at room temperature. The approach provides insight into the relative activity of early damage mechanisms in CMCs at both the surface and subsurface levels and sheds light on the impact of fabrication choices on the evolution of damage to final failure. The potential application of this combined approach towards the characterization of damage in SiC/SiC CMCs under more complex testing conditions will also be discussed.

damage evolution↗
DOE OSTI2024

A mean field homogenization model for the mechanical response of ceramic matrix composites

SiC/SiC composites offer exceptional mechanical stability at high temperatures and under irradiation. These ceramic matrix composites are therefore strong candidate materials for future nuclear energy applications. Their mechanical response, which exhibits pseudo-plasticity, is mediated by matrix cracking, fiber debonding, and fiber pull-out due to slip. Here, this study introduces a mechanistic model for the behavior of unidirectionally reinforced SiC/SiC composites. Specifically a mean field homogenization approach is proposed to account for all deformation and degradation modes during mechanical deformation. The homogenization scheme relies on a Mori Tanaka method that is extended to consider the effects of the coating’s elasto-plastic response on the development of micromechanical fields. Further, the model proposed introduces a method to effectively account for the role of localized damage (i.e., cracks) on mechanical fields within both the fiber and the matrix. Upon validating the model against experimental data, the roles of interface sliding, coating dimensions and intrinsic elastic response, as well as of microstructure (e.g. porosity, fiber volume fraction) are discussed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗