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Reliability comparisons between additively manufactured and conventional SiC–Si ceramic composites

Abstract An additively manufactured reaction‐bonded silicon carbide ceramic composite is fabricated using a bimodal powder feedstock and the binder‐jetting printing technique. On fabricating, the ceramic is investigated to report its composition, mechanical, and thermal properties at room temperature and high temperatures (up to 750). The ceramic has a density of 2.76 g/cc, and shows a hardness of 21.74 GPa, and a flexure strength of 207.5 MPa at room temperature. The mechanical property of flexure strength is used to estimate its failure probability under applied stress, using a Weibull distribution. The mechanical properties and failure probabilities are compared with those of conventionally fabricated reaction‐bonded silicon carbide ceramics reported in the literature. These ceramics were fabricated using methods such as slip‐casting, compacting, and tape‐casting. The comparison is used to elucidate the advantages and areas of improvement of the present additive manufacturing technique for reaction‐bonded ceramics.

14 SOLAR ENERGY↗

Plasma etching a ceramic composite

Plasma etching is found to be a superior metallographic technique for evaluating the microstructure of a ceramic matrix composite. The ceramic composite studied is composed of silicon carbide whiskers (SiC(sub W)) in a matrix of silicon nitride (Si3N4), glass, and pores. All four constituents are important in evaluating the microstructure of the composite. Conventionally prepared samples, both as-polished or polished and etched with molten salt, do not allow all four constituents to be observed in one specimen. As-polished specimens allow examination of the glass phase and porosity, while molten salt etching reveals the Si3N4 grain size by removing the glass phase. However, the latter obscures the porosity. Neither technique allows the SiC(sub W) to be distinguished from the Si3N4. Plasma etching with CF4 + 4 percent O2 selectively attacks the Si3N4 grains, leaving SiC(sub W) and glass in relief, while not disturbing the pores. An artifact of the plasma etching reaction is the deposition of a thin layer of carbon on Si3N4, allowing Si3N4 grains to be distinguished from SiC(sub W) by back scattered electron imaging.

Hull, David R.↗

Codes and standards for ceramic composite core materials for High Temperature Reactor applications

Fiber-reinforced ceramic matrix composites are attractive for high-temperature nuclear applications due to excellent thermal and mechanical properties as well as reasonable-to-outstanding radiation resistance. Over the past 20 years, the use of ceramic matrix composite applications expanded to many commercial non-nuclear industries as fabrication and application of the technologies mature. The ASME Boiler Pressure Vessel Code, under Section III Division 5, provides the design and construction rules for High Temperature Reactor components. It published the first rules for ceramic matrix composites to be used for reactor core components. The rules lay out the quality requirements together with the design and materials criteria for the use and application of silicon carbide- and carbon-based matrix material technologies. As with the established graphite rules, the ceramic composite material rules are structured in Subsection HH (from Section III), that addresses the criteria for class SN nonmetallic core components. The code rules rely heavily on the development and publication of standards for composite specification, classification, and testing of mechanical, thermal, and other properties. These test methods are developed in ASTM Committee C28 on Advanced Ceramics, with a current focus on ceramic composite tubes. This article describes the detail of the composites code, the design methodology and similarities to the graphite code, the guidance for the development of specifications for ceramic composites (for nuclear applications) including recent standard developments, and it mentions the next steps to support licensing aspects by validating the code with benchmarking data.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Salt ceramic composites and manufacture thereof

Highly dense lithium based ceramics can be prepared by a low temperature process including combining a lithium based ceramic with a polar solvent having a lithium based salt dissolved therein and applying pressure and heat to the combination to form a salt-ceramic composite. Advantageously, the lithium salt is one that dissolves in the polar solvent and the heat applied to the combination is no greater than about 250° C. Such composites can also have high ionic conductivity.

Gomez, Enrique Daniel↗

Reliability and effective thermal conductivity of three metallic-ceramic composite insulating coatings on cooled hydrogen-oxygen rockets

An experimental investigation of the structural integrity and effective thermal conductivity of three metallic-ceramic composite coatings was conducted. These coatings were plasma sprayed onto the combustion side of water-cooled, 12.7-centimeter throat diameter, hydrogen-oxygen rocket thrust chambers operating at 2.07 to 4.14 meganewtons per square meter chamber pressure. The metallic-ceramic composites functioned for six to 17 cycles and for as long as 213 seconds of rocket operations and could have probably provided their insulating properties for many additional cycles. The effective thermal conductivity of all the coatings was in the range of 0.7472 to 4.483 w/(m)(K), which makes the coatings a very effective thermal barrier. Photomicrographic studies of cross-sectioned coolant tubes seem to indicate that the effective thermal conductivity of the coatings is controlled by contact resistance between the particles, as a result of the spraying process, and not the thermal conductivity of the bulk materials.

Price, H. G., Jr.↗

Key Issues for Aerospace Applications of Ceramic Matrix Composites

Ceramic matrix composites (CMC) offer significant advantages for future aerospace applications including turbine engine and liquid rocket engine components, thermal protection systems, and "hot structures". Key characteristics which establish ceramic matrix composites as attractive and often enabling choices are strength retention at high temperatures and reduced weight relative to currently used metallics. However, due to the immaturity of this class of materials which is further compounded by the lack of experience with CMC's in the aerospace industry, there are significant challenges involved in the development and implementation of ceramic matrix composites into aerospace systems. Some of the more critical challenges are attachment and load transfer methodologies; manufacturing techniques, particularly scale up to large and thick section components; operational environment resistance; damage tolerance; durability; repair techniques; reproducibility; database availability; and the lack of validated design and analysis tools. The presentation will examine the technical issues confronting the application of ceramic matrix composites to aerospace systems and identify the key material systems having potential for substantial payoff relative to the primary requirements of light weight and reduced cost for future systems. Current programs and future research opportunities will be described in the presentation which will focus on materials and processes issues.

Clinton, R. G., Jr.↗

Method Developed for the High-Temperature Nondestructive Evaluation of Fiber-Reinforced Silicon Carbide Ceramic Matrix Composites

Ceramic matrix composites have emerged as candidate materials to allow higher operating temperatures (1000 to 1400 C) in gas turbine engines. A need, therefore, exists to develop nondestructive methods to evaluate material integrity at the material operating temperature by monitoring thermal and mechanical fatigue. These methods would also have potential as quality inspection tools. The goal of this investigation at the NASA Lewis Research Center is to survey and correlate the temperature-dependent damping and stiffness of advanced ceramic composite materials with imposed thermal and stress histories that simulate in-service turbine engine conditions. A typical sample size of 100 by 4 by 2 cubic millimeters, along with the specified stiffness and density, placed the fundamental vibration frequencies between 100 and 2000 Hz. A modified Forster apparatus seemed most applicable to simultaneously measure both damping and stiffness. Testing in vacuum reduced the effects of air on the measurements. In this method, a single composite sample is vibrated at its fundamental tone; then suddenly, the mechanical excitation is removed so that the sample's motion freely decays with time. Typical results are illlustrated in this paper.

Goldsby, Jon C.↗

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.↗

Theory and experimental technique for nondestructive evaluation of ceramic composites

The important ultrasonic scattering mechanisms for SiC and Si3N4 ceramic composites were identified by examining the interaction of ultrasound with individual fibers, pores, and grains. The dominant scattering mechanisms were identified as asymmetric refractive scattering due to porosity gradients in the matrix material, and symmetric diffractive scattering at the fiber-to-matrix interface and at individual pores. The effect of the ultrasonic reflection coefficient and surface roughness in the ultrasonic evaluation was highlighted. A new nonintrusive ultrasonic evaluation technique, angular power spectrum scanning (APSS), was presented that is sensitive to microstructural variations in composites. Preliminary results indicate that APSS will yield information on the composite microstructure that is not available by any other nondestructive technique.

Generazio, Edward R.↗

Energy efficient engine pin fin and ceramic composite segmented liner combustor sector rig test report

Under the NASA-sponsored Energy Efficient Engine program, Pratt and Whitney has successfully completed a comprehensive test program using a 90-degree sector combustor rig that featured an advanced two-stage combustor with a succession of advanced segmented liners. Building on the successful characteristics of the first generation counter-parallel Finwall cooled segmented liner, design features of an improved performance metallic segmented liner were substantiated through representative high pressure and temperature testing in a combustor atmosphere. This second generation liner was substantially lighter and lower in cost than the predecessor configuration. The final test in this series provided an evaluation of ceramic composite liner segments in a representative combustor environment. It was demonstrated that the unique properties of ceramic composites, low density, high fracture toughness, and thermal fatigue resistance can be advantageously exploited in high temperature components. Overall, this Combustor Section Rig Test program has provided a firm basis for the design of advanced combustor liners.

Dubiel, D. J.↗

Method of making carbon fiber-carbon matrix reinforced ceramic composites

A method of making a carbon fiber-carbon matrix reinforced ceramic composite wherein the result is a carbon fiber-carbon matrix reinforcement is embedded within a ceramic matrix. The ceramic matrix does not penetrate into the carbon fiber-carbon matrix reinforcement to any significant degree. The carbide matrix is a formed in situ solid carbide of at least one metal having a melting point above about 1850 degrees centigrade. At least when the composite is intended to operate between approximately 1500 and 2000 degrees centigrade for extended periods of time the solid carbide with the embedded reinforcement is formed first by reaction infiltration. Molten silicon is then diffused into the carbide. The molten silicon diffuses preferentially into the carbide matrix but not to any significant degree into the carbon-carbon reinforcement. Where the composite is intended to operate between approximately 2000 and 2700 degrees centigrade for extended periods of time such diffusion of molten silicon into the carbide is optional and generally preferred, but not essential.

Williams, Brian↗

Current Issues with Environmental Barrier Coatings for Ceramics and Ceramic Composites

The environmental barrier coating (EBC) for SiC/SiC ceramic matrix composites and Si3N4 ceramics is an emerging field as the application of silicon-based ceramics in the gas turbine engine hot section is on the horizon, both for aero and industrial gas turbines. EBC is an enabling technology for silicon-based ceramics because these materials without an EBC cannot be used in combustion environments due to rapid surface recession. Significant progress in EBC development has been made during the last decade through various government-sponsored programs. Current EBCs are based on silicon, mullite (3Al2O3-2SiO2) and BSAS (barium strontium aluminum silicate with celsian structure). Volatility of BSAS, BSAS-silica chemical reaction, and low melting point of silicon limit temperature capability of current EBCs to about 1350 C for long-term applications. There is a need for higher temperature EBCs as the temperature capability of silicon-based ceramics continue to increase. Therefore, research is underway to develop EBCs with improved temperature capability compared to current EBCs. The current status and issues with the advanced EBC development efforts will be discussed.

Lee, Kang N.↗

Oxidation and Corrosion of Ceramics and Ceramic Matrix Composites

Ceramics and ceramic matrix composites are candidates for numerous applications in high temperature environments with aggressive gases and possible corrosive deposits. There is a growing realization that high temperature oxidation and corrosion issues must be considered. There are many facets to these studies, which have been extensively covered in some recent reviews. The focus of this paper is on current research, over the past two years. In the authors' view, the most important oxidation and corrosion studies have focused on four major areas during this time frame. These are; (I) Oxidation of precursor-based ceramics; (II) Studies of the interphase material in ceramic matrix composites; (III) Water vapor interactions with ceramics, particularly in combustion environments; and (IV) Development of refractory oxide coatings for silicon-based ceramics. In this paper, we shall explore the most current work in each of these areas.

Jacobson, Nathan S.↗

Ultrasonic and radiographic evaluation of advanced aerospace materials: Ceramic composites

Two conventional nondestructive evaluation techniques were used to evaluate advanced ceramic composite materials. It was shown that neither ultrasonic C-scan nor radiographic imaging can individually provide sufficient data for an accurate nondestructive evaluation. Both ultrasonic C-scan and conventional radiographic imaging are required for preliminary evaluation of these complex systems. The material variations that were identified by these two techniques are porosity, delaminations, bond quality between laminae, fiber alignment, fiber registration, fiber parallelism, and processing density flaws. The degree of bonding between fiber and matrix cannot be determined by either of these methods. An alternative ultrasonic technique, angular power spectrum scanning (APSS) is recommended for quantification of this interfacial bond.

Generazio, Edward R.↗

Dynamic crack arrest in ceramics and ceramic composites

The results of past dynamic crack arrest experiments involving structural ceramics and ceramic composites are reviewed and analyzed. The lack of dynamic crack arrest in very brittle materials is discussed and contrasted with dynamic crack arrest in somewhat brittle metallic and polymeric materials. Numerical analyses show that the lack of crack arrest is due to reduced dynamic fracture resistance of the material and is not due to the kinetic energy.

Kobayashi, A. S.↗

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.↗

Composites: Processing and Fabrication Methodologies of Nonoxide Ceramic Composites. Processing HfB2 Composites for Use in Extreme Environments

HfB2 and ZrB2 composites containing SiC are known to have good thermal shock and configurational stability at elevated temperatures. These are promising ultra-high temperature ceramics (UHTCs) for use on the sharp leading edges of next generation space vehicles. Sharp leading edges on these vehicles will need to: withstand repeated exposures to temperatures > 2200 C in oxidizing environments; have good thermal shock and ablation resistance; and withstand the mechanical stress of launch and reentry. The HfB2/SiC composite is currently undergoing processing improvements in an effort to better the performance of a material that has been studied for approx. 35 years. The potential for HfB2/SiC composites to meet the requirements of hypersonic flight depends on controlling processing techniques. This presentation will focus on understanding processing steps now being undertaken to optimize the material properties of HfB2/SiC composites at NASA Ames Research Center. Correlation between processing techniques and microstructure will be shown. Preliminary oxidation studies will also be discussed.

Gusman, Michael I.↗

High Temperature Solid Particle Erosion in a Melt-Infiltrated SiC/SiC Ceramic Matrix Composite

Ceramic matrix composites (CMCs) are an enabling propulsion material system that offer weight benefits over current Ni-based superalloys, and have higher temperature capabilities that can reduce cooling requirements. Incorporating CMCs into the hot section of gas-turbine engines therefore leads to an increase in engine efficiency. While significant advancements have been made, challenges still remain for current and next-generation gas-turbines; particularly when operating in dust-laden or erosive environments. Solid particles entrained in the gas flow can impact engine hardware resulting in localized damage and material removal due to repeated, cumulative impacts. In this study, the erosion behavior of a melt-infiltrated (MI) silicon carbide fiber-reinforced silicon carbide (SiC/SiC) CMC is investigated at high temperature (1,200 °C) in a simulated combustion environment using 150 µm alumina particles as erodent. Particle impact velocities ranged from 100 to 200 m/s and the angle of impingement varied from 30° to 90°. Erosion testing was also performed on α-SiC to elucidate similarities and differences in the erosion response of the composite compared to that of a monolithic ceramic. Scanning electron microscopy (SEM) was used to study the post-erosion damage morphology and the governing mechanisms of material removal.

Ceramic matrix composites (CMCs), solid particle e↗