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NASA NTRS2018

Influence of Fiber Content, Thermal Cycles and Creep on Electrical Resistivity Measurements of SiCf/SiC Minicomposites

Fiber-reinforced Ceramic Matrix Composites (CMCs) are currently being used in high-temperature applications such as jet engine components. In such extreme environment applications, materials are exposed to many mechanical and thermal loading cycles during the life of the component. This exposure can degrade the component, and thus, components need to be monitored and inspected during service. The electrical resistivity nondestructive evaluation technique has been shown to be very sensitive to damage in CMCs, and although its performance is highly dependent on temperature, this temperature-dependence is still not well understood. Therefore, this current study aims to establish the influence of thermal cycles, creep, CVI-SiC matrix cracks and fiber volume fraction on the electrical resistance of Hi Nicalon and Hi-Nicalon Type S SiC fiber-reinforced minicomposites with BN interphases. Minicomposites with 97% CVI-SiC matrix volume fraction were used to characterize the electrical resistivity of the CVI-SiC matrix. Next, models were constructed to calculate fiber resistivity and onset and evolution of damage during tensile testing at room-temperature. The thermal cycles were achieved by heating as-received and precracked specimens to 1200Â°C and then cooling them to room temperature, with or without applied stress on fibers.

creep↗

NASA NTRS1994

System for the growth of bulk SiC crystals by modified CVD techniques

The goal of this program was the development of a SiC CVD growth of films thick enough to be useful as pseudo-substrates. The cold-walled CVD system was designed, assembled, and tested. Extrapolating from preliminary evaluation of SiC films grown in the system at relatively low temperatures indicates that the growth rate at the final temperatures will be high enough to make our approach practical. Modifications of the system to allow high temperature growth and cleaner growth conditions are in progress. This program was jointly funded by Wright Laboratory, Materials Directorate and NASA LeRC and monitored by NASA.

Steckl, Andrew J.↗

NASA NTRS2001

Packaging Technology Developed for High-Temperature Silicon Carbide Microsystems

High-temperature electronics and sensors are necessary for harsh-environment space and aeronautical applications, such as sensors and electronics for space missions to the inner solar system, sensors for in situ combustion and emission monitoring, and electronics for combustion control for aeronautical and automotive engines. However, these devices cannot be used until they can be packaged in appropriate forms for specific applications. Suitable packaging technology for operation temperatures up to 500 C and beyond is not commercially available. Thus, the development of a systematic high-temperature packaging technology for SiC-based microsystems is essential for both in situ testing and commercializing high-temperature SiC sensors and electronics. In response to these needs, researchers at Glenn innovatively designed, fabricated, and assembled a new prototype electronic package for high-temperature electronic microsystems using ceramic substrates (aluminum nitride and aluminum oxide) and gold (Au) thick-film metallization. Packaging components include a ceramic packaging frame, thick-film metallization-based interconnection system, and a low electrical resistance SiC die-attachment scheme. Both the materials and fabrication process of the basic packaging components have been tested with an in-house-fabricated SiC semiconductor test chip in an oxidizing environment at temperatures from room temperature to 500 C for more than 1000 hr. These test results set lifetime records for both high-temperature electronic packaging and high-temperature electronic device testing. As required, the thick-film-based interconnection system demonstrated low (2.5 times of the room-temperature resistance of the Au conductor) and stable (decreased 3 percent in 1500 hr of continuous testing) electrical resistance at 500 C in an oxidizing environment. Also as required, the electrical isolation impedance between printed wires that were not electrically joined by a wire bond remained high (greater than 0.4 GW) at 500 C in air. The attached SiC diode demonstrated low (less than 3.8 W/mm2) and relatively consistent dynamic resistance from room temperature to 500 C. These results indicate that the prototype package and the compatible die-attach scheme meet the initial design standards for high-temperature, low-power, and long-term operation. This technology will be further developed and evaluated, especially with more mechanical tests of each packaging element for operation at higher temperatures and longer lifetimes.

Chen, Liang-Yu↗

NASA NTRS2010

Oxidation of SiC/BN/SiC Composites in Reduced Oxygen Partial Pressures

SiC fiber-reinforced SiC composites with a BN interphase are proposed for use as leading edge structures of hypersonic vehicles. The durability of these materials under hypersonic flight conditions is therefore of interest. Thermogravimetric analysis was used to characterize the oxidation kinetics of both the constituent fibers and composite coupons at four temperatures: 816, 1149, 1343, and 1538 C (1500, 2100, 2450, and 2800 F) and in oxygen partial pressures between 5% and 0.1% (balance argon) at 1 atm total pressure. One edge of the coupons was ground off so the effects of oxygen ingress into the composite could be monitored by post-test SEM and EDS. Additional characterization of the oxidation products was conducted by XPS and TOF-SIMS. Under most conditions, the BN oxidized rapidly, leading to the formation of borosilicate glass. Rapid initial oxidation followed by volatilization of boria lead to protective oxide formation and further oxidation was slow. At 1538C in 5% oxygen, both the fibers and coupons exhibited borosilicate glass formation and bubbling. At 1538C in 0.1% oxygen, active oxidation of both the fibers and the composites was observed leading to rapid SiC degradation. BN oxidation at 1538C in 0.1% oxygen was not significant.

Opila, Elizabeth J.↗

NASA NTRS1997

Development of High Temperature Gas Sensor Technology

The measurement of engine emissions is important for their monitoring and control. However, the ability to measure these emissions in-situ is limited. We are developing a family of high temperature gas sensors which are intended to operate in harsh environments such as those in an engine. The development of these sensors is based on progress in two types of technology: (1) The development of SiC-based semiconductor technology; and (2) Improvements in micromachining and microfabrication technology. These technologies are being used to develop point-contact sensors to measure gases which are important in emission control especially hydrogen, hydrocarbons, nitrogen oxides, and oxygen. The purpose of this paper is to discuss the development of this point-contact sensor technology. The detection of each type of gas involves its own challenges in the fields of materials science and fabrication technology. Of particular importance is sensor sensitivity, selectivity, and stability in long-term, high temperature operation. An overview is presented of each sensor type with an evaluation of its stage of development. It is concluded that this technology has significant potential for use in engine applications but further development is necessary.

Hunter, Gary W.↗

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 NTRS1991

Improved silicon nitride for advanced heat engines

The results of a four year program to improve the strength and reliability of injection-molded silicon nitride are summarized. Statistically designed processing experiments were performed to identify and optimize critical processing parameters and compositions. Process improvements were monitored by strength testing at room and elevated temperatures, and microstructural characterization by optical, scanning electron microscopes, and scanning transmission electron microscope. Processing modifications resulted in a 20 percent strength and 72 percent Weibull slope improvement of the baseline material. Additional sintering aids screening and optimization experiments succeeded in developing a new composition (GN-10) capable of 581.2 MPa at 1399 C. A SiC whisker toughened composite using this material as a matrix achieved a room temperature toughness of 6.9 MPa m(exp .5) by the Chevron notched bar technique. Exploratory experiments were conducted on injection molding of turbocharger rotors.

Yeh, Harry C.↗

NASA NTRS1995

Influence of Alumina Reaction Tube Impurities on the Oxidation of Chemically-Vapor-Deposited Silicon Carbide

Pure coupons of chemically vapor deposited (CVD) SiC were oxidized for 100 h in dry flowing oxygen at 1300 C. The oxidation kinetics were monitored using thermogravimetry (TGA). The experiments were first performed using high-purity alumina reaction tubes. The experiments were then repeated using fused quartz reaction tubes. Differences in oxidation kinetics, scale composition, and scale morphology were observed. These differences were attributed to impurities in the alumina tubes. Investigators interested in high-temperature oxidation of silica formers should be aware that high-purity alumina can have significant effects on experiment results.

Opila, Elizabeth↗

NASA NTRS2010

Oxidation of SiC Fiber-Reinforced SiC Matrix Composites with a BN Interphase

SiC-fiber reinforced SiC matrix composites with a BN interphase were oxidized in reduced oxygen partial pressures of oxygen to simulate the environment for hypersonic vehicle leading edge applications. The constituent fibers as well as composite coupons were oxidized in oxygen partial pressures ranging from 1000 ppm O2 to 5% O2 balance argon. Exposure temperatures ranged from 816 C to 1353 C (1500 F to 2450 F). The oxidation kinetics of the coated fibers were monitored by thermogravimetric analysis (TGA). An initial rapid transient weight gain was observed followed by parabolic kinetics. Possible mechanisms for the transient oxidation are discussed. One edge of the composite coupon seal coat was ground off to simulate damage to the composite which allowed oxygen ingress to the interior of the composite. Oxidation kinetics of the coupons were characterized by scanning electron microscopy since the weight changes were minimal. It was found that sealing of the coupon edge by silica formation occurred. Differences in the amount and morphology of the sealing silica as a function of time, temperature and oxygen partial pressure are discussed. Implications for use of these materials for hypersonic vehicle leading edge materials are summarized.

Opila, Elizabeth↗

NASA NTRS2002

Effect of Environment on the Stress- Rupture Behavior of a C/SiC Composite Studied

Advanced reusable launch vehicles will likely incorporate fiber-reinforced ceramic matrix composites (CMC's) in critical propulsion and airframe components. The use of CMC's is highly desirable to save weight, improve reuse capability, and increase performance. One of the candidate CMC materials is carbon-fiber-reinforced silicon carbide (C/SiC). In potential propulsion applications, such as turbopump rotors and nozzle exit ramps, C/SiC components will be subjected to a service cycle that includes mechanical loading under complex, high-pressure environments containing hydrogen, oxygen, and steam. Degradation of both the C fibers and the SiC matrix are possible in these environments. The objective of this effort was to evaluate the mechanical behavior of C/SiC in various environments relevant to reusable launch vehicle applications. Stress-rupture testing was conducted at the NASA Glenn Research Center on C/SiC specimens in air and steam-containing environments. Also, the oxidation kinetics of the carbon fibers that reinforce the composite were monitored by thermogravimetric analysis in the same environments and temperatures used for the stress-rupture tests of the C/SiC composite specimens. The stress-rupture lives obtained for C/SiC tested in air and in steam/argon mixtures are shown in the following bar chart. As is typical for most materials, lives obtained at the lower temperature (600 C) are longer than for the higher temperature (1200 C). The effect of environment was most pronounced at the lower temperature, where the average test duration in steam at 600 C was at least 30 times longer than the lives obtained in air. The 1200 C data revealed little difference between the lives of specimens tested in air and steam at atmospheric pressure.

Verrilli, Michael J.↗

NASA NTRS2007

Oxidation of C/SiC Composites at Reduced Oxygen Partial Pressures

T-300 carbon fibers and T-300 carbon fiber reinforced silicon carbide composites (C/SiC) were oxidized in flowing reduced oxygen partial pressure environments at a total pressure of one atmosphere (0.5 atm O2, 0.05 atm O2 and 0.005 atm O2, balance argon). Experiments were conducted at four temperatures (816deg, 1149deg, 1343deg, and 1538 C). The oxidation kinetics were monitored using thermogravimetric analysis. T-300 fibers were oxidized to completion for times between 0.6 and 90 h. Results indicated that fiber oxidation kinetics were gas phase diffusion controlled. Oxidation rates had an oxygen partial pressure dependence with a power law exponent close to one. In addition, oxidation rates were only weakly dependent on temperature. The C/SiC coupon oxidation kinetics showed some variability, attributed to differences in the number and width of cracks in the SiC seal coat. In general, weight losses were observed indicating oxidation of the carbon fibers dominated the oxidation behavior. Low temperatures and high oxygen pressures resulted in the most rapid consumption of the carbon fibers. At higher temperatures, the lower oxidation rates were primarily attributed to crack closure due to SiC thermal expansion, rather than oxidation of SiC since these reduced rates were observed even at the lowest oxygen partial pressures where SiC oxidation is minimal.

Opila, E. J.↗

NASA NTRS2024

Development of a High Frequency Class-A Amplifier for High Temperature Wireless Microsystems based on a Silicon Carbide Static Induction Transistor

Next generation gas turbine engine health monitoring for high performance jet engine-powered aircraft will incorporate integrated microelectronic sensors specifically designed to enhance aircraft functionality, engine efficiency, and safety. Temperature, air flow and pressure associated with the gas path as well as emissions from the engine correlate to the state of the combustor and other engine health conditions. Monitoring these parameters accurately requires positioning electronic sensors in the hot zone of the gas turbine engine, which exposes them to temperatures in excess of 400ºC. At these temperatures, signal amplification is needed at the transducer level to distinguish the desired measured signal from the significant electronic noise generated by the harsh environment. In this presentation, we report on the simulation, development, fabrication, and testing on a high temperature Class-A amplifier which utilizes a 4H-SiC Static Induction Transistor (SIT) as the active device and input/output matching and DC bias networks comprised of thin-film spiral inductors, metal-insulator-metal capacitors, and thick film chip resistors. A small signal model that emulates the operation of the 4H-SiC SIT from 25 to 400ºC, with an emphasis on operation at 400οC, was utilized. Measurements were performed from 25 to 400ºC to generate current-voltage curves, capacitive transistor characteristics and high frequency scattering parameters (S-parameters). The measured data was used to extrapolate the transconductance, gm, as a function of temperature for model development. Circuit simulation tools were used to generate S-parameters, which were compared to the measured values. At 400οC, a maximum difference between measured and simulated S-parameters for frequencies from 20 to 100 MHz were 3.84%, 0.68%, 10.61%, and 3.26% for S21, S12, S11, and S22, respectively. The average transit frequency, ft, was calculated from measured values to be 197.8 MHz, while the simulated value from the model was found to be 200 MHz. The Amplifier’s S-parameters were recorded at 20-100 MHz over a temperature range of 25-400ºC and show a gain of approximately 15.8 and 5.80 dBm at 25 and 400ºC, respectively. The input and output reflection coefficients at 50 MHz and 400ºC were -18.5 and -15.2 dB, respectively. The noise figure and phase noise were measured over the temperature range of 25-400ºC and recorded. The noise figure increased 21% at 50 MHz over the temperature range, while the 1 kHz offset of the phase noise remained below -110 dB. The stability factor, K, calculated with measured and simulated data demonstrates unconditional stability over the frequency range at 400ºC. Lastly, the 1-dB compression point was measured at 50 MHz and 400ºC with an approximated output of 9.5 dBm.

SiC↗

NASA NTRS2008

Electrical Resistance of Ceramic Matrix Composites for Damage Detection and Life-Prediction

Smith, Craig↗

DOE OSTI2022

Failure evaluation of neutron-irradiated SiC/SiC composites by underwater acoustic emission

Here, understanding the statistical properties of mechanical properties of non-irradiated and neutron-irradiated SiC/SiC composites is essential for component design. This study aims to evaluate the detailed damage accumulation behavior of composites focusing on two fracture parameters: proportional limit stress (PLS) and acoustic emission (AE) onset stress. The developmental underwater AE technique, which is benefit in non-contact in-situ failure monitoring method during mechanical testing and in handle of the irradiated material, was first applied to evaluate damage accumulation behavior. Two types of chemical vapor infiltration SiC/SiC composites were used: one reinforced with Hi-Nicalon Type-S SiC fiber and one reinforced with Tyranno-SA3 SiC fiber in the form of satin-woven 2D fabrics with pyrolytic carbon interface. Neutron irradiation in the High Flux Isotope Reactor at Oak Ridge National Laboratory reached a fluence of 30 dpa at a temperature of 620–670°C. Four-point flexural tests were conducted to evaluate post-irradiation strength. Weibull statistics did not suggest marked degradation of composite strength. Detailed failure behavior evaluated by AE demonstrated no irradiation-induced change of the AE onset stress (i.e., crack initiation equivalent stress). Failure probability analysis suggests that increasing the reliability of composites (i.e., the Weibull modulus rather than strength itself) is essential to expanding the design margin and benefiting from a probabilistic design approach.

36 MATERIALS SCIENCE↗

NASA NTRS2004

NASA Tech Briefs, July 2004

Topics: Optoelectronic Sensor System for Guidance in Docking; Hybrid Piezoelectric/Fiber-Optic Sensor Sheets; Multisensor Arrays for Greater Reliability and Accuracy; Integrated-Optic Oxygen Sensors; Ka-Band Autonomous Formation Flying Sensor; CMOS VLSI Active-Pixel Sensor for Tracking; Lightweight, Self-Deploying Foam Antenna Structures; Electrically Small Microstrip Quarter-Wave Monopole Antennas; A 2-to-28-MHz Phase-Locked Loop; Portable Electromyograph; Open-Source Software for Modeling of Nanoelectronic Devices; Software for Generating Strip Maps from SAR Data; Calibration Software for use with Jurassicprok; Software for Probabilistic Risk Reduction; Software Processes SAR Motion-Measurement Data; Improved Method of Purifying Carbon Nanotubes; Patterned Growth of Carbon Nanotubes or Nanofibers; Lightweight, Rack-Mountable Composite Cold Plate/Shelves; SiC-Based Miniature High-Temperature Cantilever Anemometer; Inlet Housing for a Partial-Admission Turbine; Lightweight Thermoformed Structural Components and Optics; Growing High-Quality InAs Quantum Dots for Infrared Lasers; Selected Papers on Protoplanetary Disks; Module for Oxygenating Water without Generating Bubbles; Coastal Research Imaging Spectrometer; Rapid Switching and Modulation by use of Coupled VCSELs; Laser-Induced-Fluorescence Photogrammetry and Videogrammetry; Laboratory Apparatus Generates Dual-Species Cold Atomic Beam; Laser Ablation of Materials for Propulsion of Spacecraft; Small Active Radiation Monitor; Hybrid Image-Plane/Stereo Manipulation; Partitioning a Gridded Rectangle into Smaller Rectangles; Digital Radar-Signal Processors Implemented in FPGAs; Part 1 of a Computational Study of a Drop-Laden Mixing Layer; and Some Improvements in Signal-Conditioning Circuits.

Source record↗

NASA NTRSDate not supplied

High-Cycle Fatigue Behavior of SiC-based Ceramic Matrix Composites (CMCs) at High Temperatures

High-cycle fatigue (HCF) behavior of a melt-infiltrated, pre-preg SiC/SiC ceramic matrix composite (CMC) was investigated using dogbone tensile specimens without and with simulated cooling holes at 1500 and 2400 °F. The CMC material used for this study was fabricated by GE Aviation and had a ply configuration of [0/90/0]3. HCF tests were conducted with an R-ratio of 0.6 and a cyclic frequency of 30 Hz. Runout in HCF was defined as 30 million cycles. Monotonic tensile tests were conducted at room temperature (RT) on as-received CMC specimens and on runout HCF specimens to determine residual tensile strengths. Digital image correlation (DIC) and acoustic emission (AE) techniques were used to monitor the initiation and progression of damage in RT tensile tests on specimens with and without holes. Microscopy was performed on the polished edge of specimens without cooling holes and on the polished face of specimens with cooling holes that were tested in HCF and achieved runout. Comparisons were made with baseline specimens. Fractography was performed to examine the fracture surfaces of samples that failed under different loading conditions.

Ceramic Matrix Composites↗

DOE OSTI2022

Safety Testing of AGR-5/6/7 Compacts 2-2-2 and 2-2-4

Compacts 2-2-2 and 2-2-4 from the Advanced Gas Reactor (AGR) Fuel Development and Qualification Program’s final irradiation campaign (AGR-5/6/7) were each separately subjected to a thermal soak at 1600°C for 300 h under flowing helium to simulated conditions experienced during a postulated high-temperature gas-cooled reactor (HTGR) depressurization conduction cooldown event. The safety testing of the fuel compacts’ performance under accident conditions was conducted in the Oak Ridge National Laboratory (ORNL) Core Conduction Cooldown Test Facility (CCCTF), which utilizes a stand-alone hot cell at the Irradiated Fuels Examination Laboratory (IFEL). The CCCTF heats fuel to temperatures up to 1900°C in a non-oxidizing environment while continuously monitoring the sweep gas for radioactive 85 Kr to detect release levels associated with hermetic failure of the tristructural-isotropic (TRISO) coating surrounding each fuel kernel. In addition, certain metallic radionuclides that escape the fuel compact are collected on deposition cups that are periodically exchanged with a new cup to obtain information on the overall retention behavior of the TRISO coating layers. Because cesium can diffuse through intact pyrocarbon layers, abnormal degradation of the silicon carbide (SiC) layer in the absence of holistic TRISO coating failure is indicated by release of 134 Cs at levels equivalent to an individual particle inventory in the absence of significant 85 Kr release (Hunn et al. 2014). Additional description of the CCCTF system is provided in Appendix A.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS1999

Modal Acoustic Emission Used at Elevated Temperatures to Detect Damage and Failure Location in Ceramic Matrix Composites

Ceramic matrix composites are being developed for elevated-temperature engine applications. A leading material system in this class of materials is silicon carbide (SiC) fiber-reinforced SiC matrix composites. Unfortunately, the nonoxide fibers, matrix, and interphase (boron nitride in this system) can react with oxygen or water vapor in the atmosphere, leading to strength degradation of the composite at elevated temperatures. For this study, constant-load stress-rupture tests were performed in air at temperatures ranging from 815 to 960 C until failure. From these data, predictions can be made for the useful life of such composites under similar stressed-oxidation conditions. During these experiments, the sounds of failure events (matrix cracking and fiber breaking) were monitored with a modal acoustic emission (AE) analyzer through transducers that were attached at the ends of the tensile bars. Such failure events, which are caused by applied stress and oxidation reactions, cause these composites to fail prematurely. Because of the nature of acoustic waveform propagation in thin tensile bars, the location of individual source events and the eventual failure event could be detected accurately.

Morscher, Gregory N.↗