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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↗

NASA NTRS1998

High Temperature Mechanical Characterization of Ceramic Matrix Composites

A high temperature mechanical characterization laboratory has been assembled at NASA Lewis Research Center. One contribution of this work is to test ceramic matrix composite specimens in tension in environmental extremes. Two high temperature tensile testing systems were assembled. The systems were assembled based on the performance and experience of other laboratories and meeting projected service conditions for the materials in question. The systems use frames with an electric actuator and a center screw. A PC based data acquisition and analysis system is used to collect and analyze the data. Mechanical extensometers are used to measure specimen strain. Thermocouples, placed near the specimen, are used to measure the specimen gage section temperature. The system for testing in air has a resistance element furnace with molybdenum disilicide elements and pneumatic grips with water cooling attached to hydraulic alignment devices. The system for testing in an inert gas has a graphite resistance element furnace in a chamber with rigidly mounted, water cooled, hydraulically actuated grips. Unidirectional SiC fiber reinforced reaction bonded Si3N4 and triaxially woven, two dimensional, SiC fiber reinforced enhanced SiC composites were tested in unidirectional tension. Theories for predicting the Young's modulus, modulus near the ultimate strength, first matrix cracking stress, and ultimate strength were applied and evaluated for suitability in predicting the mechanical behavior of SiC/RBSN and enhanced SiC/SiC composites. The SiC/RBSN composite exhibited pseudo tough behavior (increased area under the stress/strain curve) from 22 C to 1500 C. The rule of mixtures provides a good estimate of the Young's modulus of the SiC/RBSN composite using the constituent properties from room temperature to 1440 C for short term static tensile tests in air or nitrogen. The rule of mixtures significantly overestimates the secondary modulus near the ultimate strength. The ACK theory provides the best approximation of the first matrix cracking stress when residual stresses are ignored. The theory of Cao and Thouless, based on Weibull statistics, gave the best prediction for the composite ultimate strength. The enhanced SiC/SiC composite exhibited nonlinear stress/strain behavior from 24 C to 1370 C in air with increased ultimate strain when compared to monolithic SiC. The theory of Yang and Chou with the assumption of a frictional fiber/matrix interface provided the best estimate of the Young's modulus. The theory of Cao and Thouless gave the best estimate for the ultimate strength.

Gyekenyesi, John Z.↗

NASA NTRS2000

Processing and Properties of SiC/MoSi2-SiC Composites Fabricated by Melt Infiltration

Hi-Nicalon SiC fiber reinforced MoSi2-SiC matrix composites (SiC/MoSi2-SiC) have been fabricated by the melt infiltration approach. The composite consists of approximately 60 vol%, 2-D woven BN/SiC coated Hi-Nicalon SiC fibers and approximately 40 vol% MoSi2-SiC matrix. The room temperature tensile properties and thermal conductivity of the SiC/MoSi2-SiC composites were measured and compared with those of the melt infiltrated SiC/SiC composites. The influence oi fiber architecture on tensile properties was also evaluated. Results indicate that the primary modulus, stress corresponding to deviation from linearity, and transverse thermal conductivity values for the SiC/MoSi2-SiC composites are significantly lower than those for the SiC/SiC composites. Microcracking of the matrix due to the large difference in thermal expansion between MoSi2 and SiC appears to be the reason for the lower matrix dominated properties of SiC/MoSi2-SiC composites.

Bhatt, Ramakrishna T.↗

NASA NTRS2001

Characterization of Ceramic Matrix Composite Combustor Components: Pre and Post Exposure

The pursuit of lower emissions and higher performance from gas turbine engines requires the development of innovative concepts and the use of advanced materials for key engine components. One key engine component is the combustor, where innovative design and material improvements have the potential to lower emissions. Efforts to develop a High Speed Civil Transport with low emissions were focused on the evaluation of combustor concepts with liners fabricated from a ceramic matrix composite of silicon carbide fibers in a silicon carbide matrix (SiC/SiC). The evaluation of SiC/SiC composites progressed from simple coupons (to establish a first-order database and identify operant failure mechanisms and damage accumulation processes), to feature-based subelements (to assess fabricability and in situ material response), to actual components (to assess structural integrity, dimensional, and compositional fidelity) tested under simulated engine conditions. As in the case of all evolutionary material and process work, a key element to resolving fabrication issues is the evaluation of witness areas taken from fabricated components before testing the actual component. The witness material from these components allowed microstructural and mechanical testing to be performed and compared to the ideal, flat panel, conditions and data that are typical of basic characterization. This also allowed samples of similar design to be taken from components after 115 hours of combustion exposure. Testing consisted of tensile, double notch shear, ring burst, and thermal conductivity that sampled various regions of the components. The evaluation of the witness material allowed an understanding of the fabrication process, highlighting critical issues, in an early phase of the learning curve development of these configuration and material unique parts. Residual property testing, after exposure, showed if degradation of the material under actual service conditions was occurring. This paper will present the results of this critical testing. Evaluations that consider the degree of complexity of the fabricated part were established to relate in situ performance to that of flat panel based coupons. Nondestructive evaluation was used throughout the evaluation process. These results will also be discussed as an aid in understanding the test results.

Ojard, G.↗

NASA NTRS2001

Environmental Barrier Coatings for Silicon-Based Ceramics

Silicon-based ceramics, such as SiC fiber-reinforced SiC (SiC/SiC ceramic matrix composites (CMC) and monolithic silicon nitride (Si3N4), are prime candidates for hot section structural components of next generation gas turbine engines. Silicon-based ceramics, however, suffer from rapid surface recession in combustion environments due to volatilization of the silica scale via reaction with water vapor, a major product of combustion. Therefore, application of silicon-based ceramic components in the hot section of advanced gas turbine engines requires development of a reliable method to protect the ceramic from environmental attack. An external environmental barrier coating (EBC) is considered a logical approach to achieve protection and CP long-term stability. The first generation EBC consisted of two layers, mullite (3Al2O3-2SiO2) bond coat and yttria-stabilized zirconia (YSZ, ZrO2-8 Wt.% Y2O3) top coat. Second generation EBCs, with substantially improved performance compared with the first generation EBC, were developed in the NASA High Speed Research-Enabling Propulsion Materials (HSR-EPM) Program. The first generation EBC consisted of two layers, mullite (3Al2O3-2SiO2) bond coat and yttria-stabilized zirconia (YSZ, ZrO2-8 wt.% Y2O3) top coat. Second generation EBCs, with substantially improved performance compared with the first generation EBC, were developed in the NASA High Speed Research-Enabling Propulsion Materials (HSR-EPM) Program (5). They consist of three layers, a silicon first bond coat, a mullite or a mullite + BSAS (BaO(1-x)-SrO(x)-Al2O3-2SiO2) second bond coat, and a BSAS top coat. The EPM EBCs were applied on SiC/SiC CMC combustor liners in three Solar Turbines (San Diego, CA) Centaur 50s gas turbine engines. The combined operation of the three engines has accumulated over 24,000 hours without failure (approximately 1,250 C maximum combustor liner temperature), with the engine in Texaco, Bakersfield, CA, accumulating about 14,000 hours. As the commercialization of Si-based ceramic components in gas turbines is on the horizon, a major emphasis is placed on EBCs for two reasons. First, they are absolute necessity for the protection of Si-based ceramics from water vapor. Second, they can enable a major enhancement in the performance of gas turbines by creating temperature gradients with the incorporation of a low thermal conductivity layer. Thorough understanding of current state-of-the-art EBCs will provide the foundation upon which development of future EBCs will be based. Phase stability and thermal conductivity of EPM EBCs are published elsewhere. This paper will discuss the chemical/environmental durability and silica volatility of EPM EBCs and their impact on the coating's upper temperature limit.

Lee, Kang N.↗

NASA NTRS2002

Characterization of Ceramic Matrix Composite Fasteners Exposed in a Combustion Liner Rig Test

Combustion tests on SiC/SiC CMC (Ceramic Matrix Composite) components were performed in an aircraft combustion environment using the Rich-burn, Quick-quench, Lean-burn (RQL) sector rig. SiC/SiC fasteners were used to attach several of these components to the metallic rig structure. The effect of combustion exposure on the fastener material was characterized via microstructural examination. Fasteners were also destructively tested, after combustion exposure, and the failure loads of fasteners exposed in the sector rig were compared to those of as-manufactured fasteners. Combustion exposure reduced the fastener failure load by 50% relative to the as-manufactured fasteners for exposure times ranging from 50 to 260 hours. The fasteners exposed in the combustion environment demonstrated failure loads that varied with failure mode. Fasteners that had the highest average failure load, failed in the same manner as the unexposed fasteners.

Verrilli, Michael J.↗

NASA NTRS2003

Nondestructive Evaluation of Ceramic Matrix Composite Combustor Components

Combustor liners fabricated from a SiC/SiC composite were nondestructively interrogated before and after combustion rig testing by X-ray, ultrasonic and thermographic techniques. In addition, mechanical test results were obtained from witness coupons, representing the as-manufactured liners, and from coupons machined from the components after combustion exposure. Thermography indications were found to correlate with reduced material properties obtained after rig testing. The thermography indications in the SiC/SiC liners were delaminations and damaged fiber tows, as determined through microstructural examinations. [copyright] 2003 American Institute of Physics

X-ray analysis↗

NASA NTRS2005

Advanced Environmental Barrier Coatings Development for Si-Based Ceramics

Advanced environmental barrier coating concepts based on multi-component HfO2 (ZrO2) and modified mullite systems are developed for monolithic Si3N4 and SiC/SiC ceramic matrix composite (CMC) applications. Comprehensive testing approaches were established using the water vapor cyclic furnace, high pressure burner rig and laser heat flux steam rig to evaluate the coating water vapor stability, cyclic durability, radiation and erosion resistance under simulated engine environments. Test results demonstrated the feasibility and durability of the environmental barrier coating systems for 2700 to 3000 F monolithic Si3N4 and SiC/SiC CMC component applications. The high-temperature-capable environmental barrier coating systems are being further developed and optimized in collaboration with engine companies for advanced turbine engine applications.

Zhu, Dong-Ming↗

NASA NTRS2004

Statistical Analysis of CMC Constituent and Processing Data

Ceramic Matrix Composites (CMCs) are the next "big thing" in high-temperature structural materials. In the case of jet engines, it is widely believed that the metallic superalloys currently being utilized for hot structures (combustors, shrouds, turbine vanes and blades) are nearing their potential limits of improvement. In order to allow for increased turbine temperatures to increase engine efficiency, material scientists have begun looking toward advanced CMCs and SiC/SiC composites in particular. Ceramic composites provide greater strength-to-weight ratios at higher temperatures than metallic alloys, but at the same time require greater challenges in micro-structural optimization that in turn increases the cost of the material as well as increases the risk of variability in the material s thermo-structural behavior. to model various potential CMC engine materials and examines the current variability in these properties due to variability in component processing conditions and constituent materials; then, to see how processing and constituent variations effect key strength, stiffness, and thermal properties of the finished components. Basically, this means trying to model variations in the component s behavior by knowing what went into creating it. inter-phase and manufactured by chemical vapor infiltration (CVI) and melt infiltration (MI) were considered. Examinations of: (1) the percent constituents by volume, (2) the inter-phase thickness, (3) variations in the total porosity, and (4) variations in the chemical composition of the Sic fiber are carried out and modeled using various codes used here at NASA-Glenn (PCGina, NASALife, CEMCAN, etc...). The effects of these variations and the ranking of their respective influences on the various thermo-mechanical material properties are studied and compared to available test data. The properties of the materials as well as minor changes to geometry are then made to the computer model and the detrimental effects observed using statistical analysis software. The ultimate purpose of this study is to determine what variations in material processing can lead to the most critical changes in the materials property. The work I have taken part in this summer explores, in general, the key properties needed In this study SiC/SiC composites of varying architectures, utilizing a boron-nitride (BN)

Fornuff, Jonathan↗

NASA NTRS2004

Characterization of Ceramic Matrix Composite Vane Subelements Subjected to Rig Testing in a Gas Turbine Environment

Vane subelements were fabricated from a silicon carbide fiber-reinforced silicon carbide matrix (SiC/SiC) composite. A cross-sectional slice of an aircraft engine metal vane was the basis of the vane subelement geometry. To fabricate the small radius of the vane's trailing edge using stiff Sylramic SiC fibers, a unique SiC fiber architecture was developed. A test configuration for the vanes in a high pressure gas turbine environment was designed and fabricated. Testing was conducted using a pressure of 6 atm and combustion flow rate of 0.5 kg/sec, and consisted of fifty hours of steady state operation followed by 102 2-minute thermal cycles. A surface temperature of 1320 C was obtained for the EBC-coated SiC/SiC vane subelement. This paper will briefly discuss the vane fabrication, test configuration, and results of the vane testing. The emphasis of the paper is on characterization of the post-test condition of the vanes.

Verrilli, Michael↗

NASA NTRS2002

Thermal Cyclic Behavior of Thermal and Environmental Barrier Coatings Investigated Under High-Heat-Flux Conditions

Environmental barrier coatings (EBC's) have been developed to protect silicon-carbide- (SiC) based ceramic components in gas turbine engines from high-temperature environmental attack. With continuously increasing demands for significantly higher engine operating temperature, future EBC systems must be designed for both thermal and environmental protection of the engine components in combustion gases. In particular, the thermal barrier functions of EBC's become a necessity for reducing the engine-component thermal loads and chemical reaction rates, thus maintaining the required mechanical properties and durability of these components. Advances in the development of thermal and environmental barrier coatings (TBC's and EBC's, respectively) will directly impact the successful use of ceramic components in advanced engines. To develop high-performance coating systems, researchers must establish advanced test approaches. In this study, a laser high-heat-flux technique was employed to investigate the thermal cyclic behavior of TBC's and EBC's on SiC-reinforced SiC ceramic matrix composite substrates (SiC/SiC) under high thermal gradient and thermal cycling conditions. Because the laser heat flux test approach can monitor the coating's real-time thermal conductivity variations at high temperature, the coating thermal insulation performance, sintering, and delamination can all be obtained during thermal cycling tests. Plasma-sprayed yttria-stabilized zirconia (ZrO2-8 wt% Y2O3) thermal barrier and barium strontium aluminosilicate-based environmental barrier coatings (BSAS/BSAS+mullite/Si) on SiC/SiC ceramic matrix composites were investigated in this study. These coatings were laser tested in air under thermal gradients (the surface and interface temperatures were approximately 1482 and 1300 C, respectively). Some coating specimens were also subject to alternating furnace cycling (in a 90-percent water vapor environment at 1300 C) and laser thermal gradient cycling tests (in air), to investigate the water vapor effect. All cyclic tests were conducted using a 60-min hot-time temperature.

Zhu, Dongming↗

NASA NTRS2004

Thermo-Mechanical Properties of Super Sylramic SiC Fibers

Ceramic matrix composites (CMC) reinforced by Sic fibers, such as SiC/SiC, are targeted for application in hot-section components of advanced engines for aerospace propulsion and for electrical power generation. Two Super Sylramic Sic fiber types recently developed at NASA using the Sylramic fiber from COI Ceramics are candidates fof providing these components with improved thermal capability and improved performance. This paper reports on the state-of-the-art ability of these new fiber types to meet the key fiber requirements of these applications: high strength, high creep-rupture resistance, high environmental resistance, and high thermal conductivity. For example, creep-rupture tests performed at from 1350 to 1500 C under various environments to simulate CMC fabrication and service conditions show creep resistance in air improved -20 and -7 times in comparison to current Sylramic and Sylramic-iBN fiber types, respectively. This in turn resulted in an increase in fiber rupture life by up to two orders of magnitude. TEM and AES microscopic observations are presented to indicate that these improvements can be correlated with the replacement of weak grain boundary phases with stronger phases that hinder grain boundary sliding more effectively. SiC/SiC composite results are also provided to show the advantages of the Super Sylramic fiber types both for CMC fabrication and high temperature application.

Yun, H. M.↗

NASA NTRS2007

Improving Turbine Performance with Ceramic Matrix Composites

Under the new NASA Fundamental Aeronautics Program, efforts are on-going within the Supersonics Project aimed at the implementation of advanced SiC/SiC ceramic composites into hot section components of future gas turbine engines. Due to recent NASA advancements in SiC-based fibers and matrices, these composites are lighter and capable of much higher service temperatures than current metallic superalloys, which in turn will allow the engines to operate at higher efficiencies and reduced emissions. This presentation briefly reviews studies within Task 6.3.3 that are primarily aimed at developing physics-based concepts, tools, and process/property models for micro- and macro-structural design, fabrication, and lifing of SiC/SiC turbine components in general and airfoils in particular. Particular emphasis is currently being placed on understanding and modeling (1) creep effects on residual stress development within the component, (2) fiber architecture effects on key composite properties such as design strength, and (3) preform formation processes so that the optimum architectures can be implemented into complex-shaped components, such as turbine vanes and blades.

DiCarlo, James A.↗

NASA NTRS2008

Monitoring Damage Accumulation in Ceramic Matrix Composites Using Electrical Resistivity

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

Smith, Craig E.↗

NASA NTRS2003

Nondestructive Evaluation of Ceramic Matrix Composite Combustor Components

Combustor liners fabricated from a SiC/SiC composite (silicon carbide fibers in a silicon carbide matrix) were nondestructively interrogated before and after combustion rig testing by x-ray, ultrasonic, and thermographic techniques. In addition, mechanical test results were obtained from witness coupons, representing the as-manufactured liners, and from coupons machined from the components after combustion exposure. Thermography indications correlated with reduced material properties obtained after rig testing. The thermography indications in the SiC/SiC liners were delaminations and damaged fiber tows, as determined through microstructural examinations.

Sun, Jiangang G.↗

NASA NTRS2010

Economical Fabrication of Thick-Section Ceramic Matrix Composites

A method was developed for producing thick-section [>2 in. (approx.5 cm)], continuous fiber-reinforced ceramic matrix composites (CMCs). Ultramet-modified fiber interface coating and melt infiltration processing, developed previously for thin-section components, were used for the fabrication of CMCs that were an order of magnitude greater in thickness [up to 2.5 in. (approx.6.4 cm)]. Melt processing first involves infiltration of a fiber preform with the desired interface coating, and then with carbon to partially densify the preform. A molten refractory metal is then infiltrated and reacts with the excess carbon to form the carbide matrix without damaging the fiber reinforcement. Infiltration occurs from the inside out as the molten metal fills virtually all the available void space. Densification to <5 vol% porosity is a one-step process requiring no intermediate machining steps. The melt infiltration method requires no external pressure. This prevents over-infiltration of the outer surface plies, which can lead to excessive residual porosity in the center of the part. However, processing of thick-section components required modification of the conventional process conditions, and the means by which the large amount of molten metal is introduced into the fiber preform. Modification of the low-temperature, ultraviolet-enhanced chemical vapor deposition process used to apply interface coatings to the fiber preform was also required to accommodate the high preform thickness. The thick-section CMC processing developed in this work proved to be invaluable for component development, fabrication, and testing in two complementary efforts. In a project for the Army, involving SiC/SiC blisk development, nominally 0.8 in. thick x 8 in. diameter (approx. 2 cm thick x 20 cm diameter) components were successfully infiltrated. Blisk hubs were machined using diamond-embedded cutting tools and successfully spin-tested. Good ply uniformity and extremely low residual porosity (<2 percent) were achieved, the latter being far lower than that achieved with SiC matrix composites fabricated via CVI or PIP. The pyrolytic carbon/zirconium nitride interface coating optimized in this work for use on carbon fibers was incorporated in the SiC/SiC composites and yielded a >41 ksi (approx. 283 MPa) flexural strength.

Babcock, Jason↗

NASA NTRS2011

Physics-Based Design Tools for Lightweight Ceramic Composite Turbine Components with Durable Microstructures

Under the Supersonics Project of the NASA Fundamental Aeronautics Program, modeling and experimental efforts are underway to develop generic physics-based tools to better implement lightweight ceramic matrix composites into supersonic engine components and to assure sufficient durability for these components in the engine environment. These activities, which have a crosscutting aspect for other areas of the Fundamental Aero program, are focusing primarily on improving the multi-directional design strength and rupture strength of high-performance SiC/SiC composites by advanced fiber architecture design. This presentation discusses progress in tool development with particular focus on the use of 2.5D-woven architectures and state-of-the-art constituents for a generic un-cooled SiC/SiC low-pressure turbine blade.

DiCarlo, James A.↗