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NASA NTRS2004

High-Performance SiC/SiC Ceramic Composite Systems Developed for 1315 C (2400 F) Engine Components

As structural materials for hot-section components in advanced aerospace and land-based gas turbine engines, silicon carbide (SiC) ceramic matrix composites reinforced by high performance SiC fibers offer a variety of performance advantages over current bill-of-materials, such as nickel-based superalloys. These advantages are based on the SiC/SiC composites displaying higher temperature capability for a given structural load, lower density (approximately 30- to 50-percent metal density), and lower thermal expansion. These properties should, in turn, result in many important engine benefits, such as reduced component cooling air requirements, simpler component design, reduced support structure weight, improved fuel efficiency, reduced emissions, higher blade frequencies, reduced blade clearances, and higher thrust. Under the NASA Ultra-Efficient Engine Technology (UEET) Project, much progress has been made at the NASA Glenn Research Center in identifying and optimizing two highperformance SiC/SiC composite systems. The table compares typical properties of oxide/oxide panels and SiC/SiC panels formed by the random stacking of balanced 0 degrees/90 degrees fabric pieces reinforced by the indicated fiber types. The Glenn SiC/SiC systems A and B (shaded area of the table) were reinforced by the Sylramic-iBN SiC fiber, which was produced at Glenn by thermal treatment of the commercial Sylramic SiC fiber (Dow Corning, Midland, MI; ref. 2). The treatment process (1) removes boron from the Sylramic fiber, thereby improving fiber creep, rupture, and oxidation resistance and (2) allows the boron to react with nitrogen to form a thin in situ grown BN coating on the fiber surface, thereby providing an oxidation-resistant buffer layer between contacting fibers in the fabric and the final composite. The fabric stacks for all SiC/SiC panels were provided to GE Power Systems Composites for chemical vapor infiltration of Glenn designed BN fiber coatings and conventional SiC matrices. Composite panels with system B were heat treated at Glenn, and the pores that remained open were filled by silicon melt infiltration (MI). Panels with system A and the other SiC/SiC systems were not heat treated, and remaining open pores in these systems were filled with SiC slurry and silicon MI.

DiCarlo, James A.↗

NASA NTRS2000

Affordable, Robust Ceramic Joining Technology (ARCJoinT) Given 1999 R and D 100 Award

Advanced ceramics and fiber-reinforced ceramic matrix composites with high strength and toughness, good thermal conductivity, thermal shock resistance, and oxidation resistance are needed for high-temperature structural applications in advanced high-efficiency and high-performance engines, space propulsion components, and land-based systems. The engineering designs of these systems require the manufacturing of large parts with complex shapes, which are either quite expensive or impossible to fabricate. In many instances, it is more economical to build complex shapes by joining together simple geometrical shapes. Thus, joining has been recognized as an enabling technology for the successful utilization of advanced ceramics and fiber-reinforced composite components in high-temperature applications. However, such joints must retain their structural integrity at high temperatures and must have mechanical strength and environmental stability comparable to those of the bulk materials. In addition, the joining technique should be robust, practical, and reliable. ARCJoinT, which is based on the reaction-forming approach, is unique in terms of producing joints with tailorable microstructures. The formation of joints by this approach is attractive since the thermomechanical properties of the joint interlayer can be tailored to be very close to those of the base materials. In addition, high-temperature fixturing is not needed to hold the parts at the infiltration temperature. The joining process begins with the application of a carbonaceous mixture in the joint area, holding the items to be joined in a fixture, and curing at 110 to 120 C for 10 to 20 min. This step fastens the pieces together. Then, silicon or a silicon alloy in tape, paste, or slurry form is applied around the joint region and heated to 1250 to 1425 C (depending on the type of infiltrant) for 10 to 15 min. The molten silicon or silicon-refractory metal alloy reacts with carbon to form silicon carbide with controllable amounts of silicon and other phases as determined by the alloy composition. Joint thickness can be readily controlled through adjustments of the properties of the carbonaceous paste and the applied fixturing force. The photograph shows various shapes of silicon-carbide-based ceramics and fiberreinforced composites that have been joined using ARCJoinT. Thermomechanical and thermochemical characterization of joints is underway for a wide variety of silicon-carbidebased advanced ceramics and fiber-reinforced composites under the hostile environments that will be encountered in engine applications. ARCJoinT, which was developed by researchers at the NASA Glenn Research Center at Lewis Field, received R&D Magazine's prestigious R&D 100 Award in 1999.

Singh, Mrityunjay↗

NASA NTRS2004

Thermo-Mechanical Properties of SiC/SiC Composites with Hybrid CVI-PIP Matrices

For long term structural service, the upper temperature capability for slurry-cast melt infiltrated (MI) SiC/SiC composites is limited to approx. 1315 C because of silicon reaction with the SiC fibers. For applications requiring material temperatures in excess of 1315 C, alternate methods of manufacturing the SiC matrices without silicon are being investigated, such as a hybrid combination of CVI and PIP. In this study, stacked fabric plies of Sylramic i-BN SiC fibers were coated with a CVI BN interface layer followed by a partial CVI SiC matrix. The remaining porosity in the SiC/SiC preforms was then infiltrated with silicon carbide matrix by PIP. Thermo-mechanical property measurements indicate that these composites are stable to 1700 C in inert environments under no load conditions for 100 h and under load conditions to 1450 C in air for 300 h. The advantages, disadvantages, and potential of this composite system for high temperature applications will be discussed.

Bhatt, R. T.↗

NASA NTRS2000

Article and method for making complex shaped preform and silicon carbide composite by melt infiltration

Small diameter silicon carbide-containing fibers are provided in a bundle such as a fiber tow that can be formed into a structure where the radii of curvature is not limited to 10-20 inches. An aspect of this invention is directed to impregnating the bundles of fibers with the slurry composition to substantially coat the outside surface of an individual fiber within the bundle and to form a complex shaped preform with a mass of continuous fibers.

Steibel, James D.↗

NASA NTRS1998

Process for making silicon carbide reinforced silicon carbide composite

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

Lau, Sai-Kwing↗

NASA NTRS2001

Article and method for making complex shaped preform and silicon carbide composite by melt infiltration

Steibel, James D.↗

NASA NTRS2001

Silicon carbide reinforced silicon carbide composite

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

Lau, Sai-Kwing↗

NASA NTRS2008

Tensile Creep and Fatigue of Sylramic-iBN Melt-Infiltrated SiC Matrix Composites: Retained Properties, Damage Development, and Failure Mechanisms

An understanding of the elevated temperature tensile creep, fatigue, rupture, and retained properties of ceramic matrix composites (CMC) envisioned for use in gas turbine engine applications are essential for component design and life-prediction. In order to quantify the effect of stress, time, temperature, and oxidation for a state-of-the-art composite system, a wide variety of tensile creep, dwell fatigue, and cyclic fatigue experiments were performed in air at 1204 C for the SiC/SiC CMC system consisting of Sylramic-iBN SiC fibers, BN fiber interphase coating, and slurry-cast melt-infiltrated (MI) SiC-based matrix. Tests were either taken to failure or interrupted. Interrupted tests were then mechanically tested at room temperature to determine the residual properties. The retained properties of most of the composites subjected to tensile creep or fatigue were usually within 20% of the as-produced strength and 10% of the as-produced elastic modulus. It was observed that during creep, residual stresses in the composite are altered to some extent which results in an increased compressive stress in the matrix upon cooling and a subsequent increased stress required to form matrix cracks. Microscopy of polished sections and the fracture surfaces of specimens which failed during stressed-oxidation or after the room-temperature retained property test was performed on some of the specimens in order to quantify the nature and extent of damage accumulation that occurred during the test. It was discovered that the distribution of stress-dependent matrix cracking at 1204 C was similar to the as-produced composites at room temperature; however, matrix crack growth occurred over time and typically did not appear to propagate through thickness except at final failure crack. Failure of the composites was due to either oxidation-induced unbridged crack growth, which dominated the higher stress regime (> 179 MPa) or controlled by degradation of the fibers, probably caused by intrinsic creep-induced flaw growth of the fibers or internal attack of the fibers via Si diffusion through the CVI SiC and/or microcracks at the lower stress regime (< 165 MPa).

Morscher, Greg↗

NASA NTRS2001

Methods for providing ceramic matrix composite components with increased thermal capacity

A method for enhancing the cooling capability of a turbine component made from a ceramic matrix composite. The method improves the thermal performance of the component by producing a surface having increased cooling capacity, thereby allowing the component to operate at a higher temperature. The method tailors the available surface area on the cooling surface of the composite component by depositing a particulate layer of coarse grained ceramic powders of preselected size onto the surface of the ceramic matrix composite component. The size of the particulate is selectively tailored to match the desired surface finish or surface roughness of the article. The article may be designed to have different surface finishes for different locations, so that the application of different sized powders can provide different cooling capabilities at different locations, if desired. The compositions of the particulates are chemically compatible with the ceramic material comprising the outer surface or portion of the ceramic matrix composite. The particulates are applied using a slurry and incorporated into the article by heating to an elevated temperature without melting the matrix, the particulates or the fiber reinforcement.

Steibel, James Dale↗

NASA NTRS2006

Hubble Space Telescope 2004 Battery Update

Battery cell wear out mechanisms and signatures are examined and compared to orbital data from the six on-orbit Hubble Space Telescope (HST) batteries, and the Flight Spare Battery (FSB) Test Bed at Marshall Space Flight Center (MSFC), which is instrumented with individual cell voltage monitoring. The on-orbit HST batteries were manufactured on an expedited basis after the Challenger Shuttle Disaster in 1986. The original design called for the HST to be powered by six 50 Ah Nickel Cadmium batteries, which would have required a shuttle mission every 5 years for battery replacement. The decision to use NiH2 instead has resulted in a longer life battery set which was launched with HST in April 1990, with a design life of 7 years that has now exceeded 14+ years of orbital cycling. This chart details the specifics of the original HST NiH2 cell design. The HST replacement batteries for Service Mission 4, originally scheduled for Spring 2005, are currently in cold storage at NASA Goddard Space Flight Center (GSFC). The SM4 battery cells utilize slurry process electrodes having 80% porosity.

Hollandsworth, Roger↗

NASA NTRS2008

Evaluation of Perfluoropolyether Lubricant Lifetime in the High Stress and High Stress-Cycle Regime for Mars Applications

The successful operation of long-life, highly loaded mechanisms used for planetary exploration or autonomous structures assembly will depend upon the ability to effectively lubricate rolling-element bearings. As new tools are developed (i.e., drill, abraders, robotic manipulators, etc.) that interact with their environment in a more direct manner, lubricants will be pushed past the bounds that current scientific literature has published. This paper details results from bearing lubrication lifetime testing performed in support of Honeybee Robotics development of the Mars Science Laboratory (MSL) Surface Removal Tool (SRT). This testing was done due to the lack of available data in research literature that is applicable to the lubrication regime the SRT bearings are being designed for. Based on the test results, the chosen bearing arrangement can be used for the SRT Grind Shaft bearings with the use of a Braycote Micronic 601EF grease-plate with a 10 vol% grease slurry fill (50/50 wt% Braycote Micronic 601EF and Brayco 815Z). This arrangement showed no signs of detrimental degradation over the course of the 3x life test. The purely grease-plated bearing ran at a consistently higher torque and showed signs of failure beginning at approximately 2.2 x 10(exp 7) revs (approximately 6.3 x 10(exp 7) stress-cycles) with a torque over-limit failure at approximately 4.5 x 10(exp 7) revs (approximately 1.3 x 10(exp 8) stress-cycles). Barring cold-start torque margin limitations, it is recommended that any long-life bearing application include some vol% grease-pack in addition to a standard grease-plate to reduce parasitic torque and increase bearing life. While these results are specific to a particular environment and loading condition, they demonstrate the extended capabilities of a commonly used flight lubricant outside of the range that is published in current research literature.

Herman, Jason↗

NASA NTRS2008

SiC/SiC Composites: The Effect of Fiber Type and Fiber Architecture on Mechanical Properties

Woven SiC/SiC composites represent a broad family of composites with a broad range of properties which are of interest for many energy-based and aero-based applications. Two important features of SiC/SiC composites which one must consider are the reinforcing fibers themselves and the fiber-architecture they are formed into. The range of choices for these two features can result in a wide range of elastic, mechanical, thermal, and electrical properties. In this presentation, it will be demonstrated how the effect of fiber-type and fiber architecture effects the important property of "matrix cracking stress" for slurry-cast melt-infiltrated SiC matrix composites, which is often considered to be a critical design parameter for this system of composites.

Morscher, Gregory N.↗

NASA NTRS2007

Improved High-Voltage Gas Isolator for Ion Thruster

A report describes an improved high-voltage isolator for preventing electrical discharge along the flow path of a propellant gas being fed from a supply at a spacecraft chassis electrical potential to an ion thruster at a potential as high as multiple kilovolts. The isolator must survive launch vibration and must remain electrically nonconductive for thousands of hours under conditions that, in the absence of proper design, would cause formation of electrically conductive sputtered metal, carbon, and/or decomposed hydrocarbons on its surfaces. The isolator includes an alumina cylinder containing a spiral channel filled with a porous medium made from alumina microbeads fired together with an alumina slurry. Connections to gas-transport tubes are made at both ends of the alumina cylinder by means of metal caps containing fine-mesh screens to prevent passage of loose alumina particles. The outer surface of the alumina cylinder is convoluted to lengthen the electrical path between the metal caps and to afford shadow shielding to minimize the probability of formation of a continuous deposit that would electrically connect the ends. A flanged cylindrical metal cap that surrounds the alumina cylinder without touching one of the ends provides additional shadow shielding.

Banks, Bruce↗

NASA NTRS2009

Application of a mixed metal oxide catalyst to a metallic substrate

A method for applying a mixed metal oxide catalyst to a metallic substrate for the creation of a robust, high temperature catalyst system for use in decomposing propellants, particularly hydrogen peroxide propellants, for use in propulsion systems. The method begins by forming a prepared substrate material consisting of a metallic inner substrate and a bound layer of a noble metal intermediate. Alternatively, a bound ceramic coating, or frit, may be introduced between the metallic inner substrate and noble metal intermediate when the metallic substrate is oxidation resistant. A high-activity catalyst slurry is applied to the surface of the prepared substrate and dried to remove the organic solvent. The catalyst layer is then heat treated to bind the catalyst layer to the surface. The bound catalyst layer is then activated using an activation treatment and calcinations to form the high-activity catalyst system.

Sevener, Kathleen M.↗

NASA NTRS2009

Method for one-to-one polishing of silicon nitride and silicon oxide

The present invention provides a method of removing silicon nitride at about the same removal rate as silicon dioxide by CMP. The method utilizes a polishing slurry that includes colloidal silica abrasive particles dispersed in water and additives that modulate the silicon dioxide and silicon nitride removal rates such that they are about the same. In one embodiment of the invention, the additive is lysine or lysine mono hydrochloride in combination with picolinic acid, which is effective at a pH of about 8. In another embodiment of the invention, the additive is arginine in combination with picolinic acid, which is effective at a pH of about 10.

Babu, Suryadevara V.↗

NASA NTRS2010

Automated Desalting Apparatus

Because salt and metals can mask the signature of a variety of organic molecules (like amino acids) in any given sample, an automated system to purify complex field samples has been created for the analytical techniques of electrospray ionization/ mass spectroscopy (ESI/MS), capillary electrophoresis (CE), and biological assays where unique identification requires at least some processing of complex samples. This development allows for automated sample preparation in the laboratory and analysis of complex samples in the field with multiple types of analytical instruments. Rather than using tedious, exacting protocols for desalting samples by hand, this innovation, called the Automated Sample Processing System (ASPS), takes analytes that have been extracted through high-temperature solvent extraction and introduces them into the desalting column. After 20 minutes, the eluent is produced. This clear liquid can then be directly analyzed by the techniques listed above. The current apparatus including the computer and power supplies is sturdy, has an approximate mass of 10 kg, and a volume of about 20 20 20 cm, and is undergoing further miniaturization. This system currently targets amino acids. For these molecules, a slurry of 1 g cation exchange resin in deionized water is packed into a column of the apparatus. Initial generation of the resin is done by flowing sequentially 2.3 bed volumes of 2N NaOH and 2N HCl (1 mL each) to rinse the resin, followed by .5 mL of deionized water. This makes the pH of the resin near neutral, and eliminates cross sample contamination. Afterward, 2.3 mL of extracted sample is then loaded into the column onto the top of the resin bed. Because the column is packed tightly, the sample can be applied without disturbing the resin bed. This is a vital step needed to ensure that the analytes adhere to the resin. After the sample is drained, oxalic acid (1 mL, pH 1.6-1.8, adjusted with NH4OH) is pumped into the column. Oxalic acid works as a chelating reagent to bring out metal ions, such as calcium and iron, which would otherwise interfere with amino acid analysis. After oxalic acid, 1 mL 0.01 N HCl and 1 mL deionized water is used to sequentially rinse the resin. Finally, the amino acids attached to the resin, and the analytes are eluted using 2.5 M NH4OH (1 mL), and the NH4OH eluent is collected in a vial for analysis.

Spencer, Maegan K.↗

NASA NTRS2010

Mud Volcanoes - Analogs to Martian Cones and Domes (by the Thousands!)

Mud volcanoes are mounds formed by low temperature slurries of gas, liquid, sediments and rock that erupt to the surface from depths of meters to kilometers. They are common on Earth, with estimates of thousands onshore and tens of thousands offshore. Mud volcanoes occur in basins with rapidly-deposited accumulations of fine-grained sediments. Such settings are ideal for concentration and preservation of organic materials, and mud volcanoes typically occur in sedimentary basins that are rich in organic biosignatures. Domes and cones, cited as possible mud volcanoes by previous authors, are common on the northern plains of Mars. Our analysis of selected regions in southern Acidalia Planitia has revealed over 18,000 such features, and we estimate that more than 40,000 occur across the area. These domes and cones strongly resemble terrestrial mud volcanoes in size, shape, morphology, associated flow structures and geologic setting. Geologic and mineralogic arguments rule out alternative formation mechanisms involving lava, ice and impacts. We are studying terrestrial mud volcanoes from onshore and submarine locations. The largest concentration of onshore features is in Azerbaijan, near the western edge of the Caspian Sea. These features are typically hundreds of meters to several kilometers in diameter, and tens to hundreds of meters in height. Satellite images show spatial densities of 20 to 40 eruptive centers per 1000 square km. Many of the features remain active, and fresh mud flows as long as several kilometers are common. A large field of submarine mud volcanoes is located in the Gulf of Cadiz, off the Atlantic coasts of Morocco and Spain. High-resolution sonar bathymetry reveals numerous km-scale mud volcanoes, hundreds of meters in height. Seismic profiles demonstrate that the mud erupts from depths of several hundred meters. These submarine mud volcanoes are the closest morphologic analogs yet found to the features in Acidalia Planitia. We are also conducting laboratory analyses of surface samples collected from mud volcanoes in Azerbaijan, Taiwan and Japan. X-ray diffraction, visible / near infrared reflectance spectroscopy and Raman spectroscopy show that the samples are dominated by mixed-layer smectite clays, along with quartz, calcite and pyrite. Thin section analysis by optical and scanning electron microscopy confirms the mineral identifications. These samples also contain chemical and morphological biosignatures, including common microfossils, with evidence of partial replacement by pyrite. The bulk samples contain approximately 1 wt% total organic carbon and 0.4 mg / gm volatile hydrocarbons. The thousands of features in Acidalia Planitia cited as analogous to terrestrial mud volcanoes clearly represent an important element in the sedimentary record of Mars. Their location, in the distal depocenter for massive Hesperian-age floods, suggests that they contain fine-grained sediments from a large catchment area in the martian highlands. We have proposed these features as a new class of exploration target that can provide access to minimally-altered material from significant depth. By analogy to terrestrial mud volcanoes, these features may also be excellent sites for the sampling martian organics and subsurface microbial life, if such exist or ever existed.

Allen, Carlton C.↗

NASA NTRS2006

SiC Composite Turbine Vanes

Turbine inlet guide vanes have been fabricated from composites of silicon carbide fibers in silicon carbide matrices. A unique design for a cloth made from SiC fibers makes it possible to realize the geometric features necessary to form these vanes in the same airfoil shapes as those of prior metal vanes. The fiber component of each of these vanes was made from SiC-fiber cloth coated with boron nitride. The matrix was formed by chemical-vapor infiltration with SiC, then slurry-casting of SiC, followed by melt infiltration with silicon. These SiC/SiC vanes were found to be capable of withstanding temperatures 400 F (222 C) greater than those that can be withstood by nickel-base-superalloy turbine airfoils now in common use in gas turbine engines. The higher temperature capability of SiC/SiC parts is expected to make it possible to use them with significantly less cooling than is used for metallic parts, thereby enabling engines to operate more efficiently while emitting smaller amounts of NOx and CO. The SiC/SiC composite vanes were fabricated in two different configurations. Each vane of one of the configurations has two internal cavities formed by a web between the suction and the pressure sides of the vane. Each vane of the other configuration has no web (see Figure 1). It is difficult to fabricate components having small radii, like those of the trailing edges of these vanes, by use of stiff stoichiometric SiC fibers currently preferred for SiC/SiC composites. To satisfy the severe geometric and structural requirements for these vanes, the aforementioned unique cloth design, denoted by the term Y-cloth, was conceived (see Figure 2). In the regions away from the trailing edge, the Y-cloth features a fiber architecture that had been well characterized and successfully demonstrated in combustor liners. To form a sharp trailing edge (having a radius of 0.3 mm), the cloth was split into two planes during the weaving process. The fiber tows forming the trailing-edge section were interlocked, thereby enhancing through-thickness strength of the resulting composite material. For vanes of the webless configuration, each made from a layup of six plies of Ycloth, the length of each Y-cloth layer was cut so that the two strips corresponding to the aforementioned two planes would wrap around the perimeter of a graphite vane preform tool with a 10-mm overlap. The overlap was used to join the two strips in a fringe splice. To make the external sixth ply, a standard woven cloth was cut to the required final length and a fringe splice joined the two ends of the cloth at the trailing edge. The cloth was then prepregged. The entire assembly was then placed into an aluminum compaction tool designed to form the outer net shape of the vane. After the prepreg material was allowed to dry, the preform was removed from the aluminum tooling and placed into an external graphite tool before being shipped to a vendor for matrix infiltration. To make the SiC fiber preform for a vane having an internal web, a slightly different initial approach was followed. Each of two sections forming the internal cavities (and ultimately the web) was created by first slipping two concentric layers of a two-dimensional, 2-by-2, 45 - braided tube around a net-shape graphite mandrel. The tubes on both mandrels were prepregged and allowed to dry. The resulting two subassemblies were put together, then four additional plies were wrapped around them in the same fashion as that described above for the six plies of the vaneless configuration. The consolidation of the SiC fiber preforms into SiC/SiC composite parts was performed by commercial vendors using their standard processes. The capability of two of the webless SiC/SiC turbine vanes was demonstrated in tests in a turbine environment. The tests included 50 hours of steady-state operation and 102 two-minute thermal cycles. A surface temperature of 1,320 C was reached during the tests.

Calomino, Anthony M.↗