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NASA NTRS1998

Oxidation of Chemically-Vapor-Deposited Silicon Carbide in Carbon Dioxide

Chemically-vapor-deposited silicon carbide (CVD SiC) was oxidized in carbon dioxide (CO2) at temperatures of 1200-1400 C for times between 96 and 500 h at several gas flow rates. Oxidation weight gains were monitored by thermogravimetric analysis (TGA) and were found to be very small and independent of temperature. Possible rate limiting kinetic mechanisms are discussed. Passive oxidation of SiC by CO2 is negligible compared to the rates measured for other oxidants that are also found in combustion environments, oxygen and water vapor.

Opila, Elizabeth J.↗

NASA NTRS2004

High-Temperature Probe Station Developed to Characterize Microwave Devices Through 500 C

A photograph and a block diagram of the high-temperature probe station are shown. The system consists of the ceramic heater mounted on a NASA shuttle tile insulator, a direct current power supply, a personal-computer-based data acquisition and temperature controller, microwave probes, a microscope, and a network analyzer. The ability to perform microwave tests at high temperatures is becoming necessary. There is now a need for sensors and communication circuits that can operate at 500 C and above for aircraft engine development and monitoring during flight. To address this need, researchers have fabricated devices using wide bandgap semiconductors such as SiC with targeted operating temperatures of 500 to 600 C. However, the microwave properties of these devices often change drastically with temperature, so any designs that are intended to be used in such an environment must be characterized at high temperatures. For some reliability, lifetime, and direct-current testing, the device under test can be packaged and characterized in an oven. However, for RF and microwave measurements, it is usually not possible to establish a calibrated reference plane at the device terminals within a package. In addition, the characteristics of the package would vary over a 500 C temperature range, and this would have to be accounted for when the data were analyzed. A high temperature probe station allows circuits and devices to be characterized through on wafer measurements across a broad temperature range with known reference plane. The conventional, commercially available thermal wafer-probe stations that are used to evaluate microwave devices across a controlled temperature range have a typical upper limit of 200 C. Standalone thermal heating chucks are available with an extended upper temperature range of 300 to 400 C. To effectively characterize devices at temperatures up to and surpassing 500 C, Glenn researchers developed a custom probe station. In the past, custom probe stations have been developed to test devices under other extreme environments, such as cryogenic temperatures as low as 37 K. Similarly, this custom probe station was specifically modified for high-temperature use. It allows devices to be measured quickly and flexibly, without the use of wire bonds and test fixtures. The probe station is shown making scattering parameter measurements from 1 to 50 GHz with a Hewlett-Packard 8510C Network Analyzer. There is a half-wafer of silicon directly on top of the heater to provide a uniform heated platform for our sample. A quarter wafer of silicon carbide forms the substrate for our test circuit of several transmission lines.

Downey, Alan N.↗

NASA NTRS1992

Failure mechanisms of 3-D woven SiC/SiC composites under tensile and flexural loading at room and elevated temperatures

Nicalon silicon carbide 3D yarn with silicon carbide matrix composites made through a chemical vapor infiltration (CVI) process were investigated under tensile and flexural loading at 23, 1200 and 1550 C in air. The effectiveness of a chemical vapor deposition (CVD) SiC surface coating was also evaluated in severe oxidizing environment. Acoustic emission sensors and in situ optical microscopy were used at room temperature to monitor the failure mechanisms. It is shown that the level of tensile stress at which nonlinear behavior begins is not drastically reduced at 1200 and 1550 C when composites were protected by a SiC surface coating. Extensive fiber pull-out was observed only in the 1550 C specimen. Similar behaviors were also found in flexural specimens.

Chulya, Abhisak↗

NASA NTRS1998

Modal Acoustic Emission of Damage Accumulation in Woven SiC/SiC at Elevated Temperatures

Ceramic matrix composites exhibit significant nonlinear stress-strain behavior that makes them attractive as potential materials for many high temperature applications. The mechanisms for this nonlinear stress-strain behavior are all associated with various types of damage in the composites, e.g. transverse matrix cracks and individual fiber failures. Modal acoustic emission has been employed to aid in discerning the damage accumulation that occurs during elevated temperature tensile stress-rupture of woven Hi-Nicalon fiber, BN interphase, SiC matrix composites. It is shown that modal acoustic emission is an effective monitor of the relative damage accumulation in the composites and locator of the damage and failure events as a function of strain (stress), time at temperature, and temperature gradients along the length of the elevated temperature test specimen.

Morscher, G. N.↗

NASA NTRS2001

Palladium Implanted Silicon Carbide for Hydrogen Sensing

Silicon carbide is intended for use in fabrication of high-temperature, efficient hydrogen sensors. Traditionally, when a palladium coating is applied on the exposed surface of SiC, the chemical reaction between palladium and hydrogen produces a detectable change in the surface chemical potential. We have produced both a palladium coated SiC as well as a palladium, ion implanted SiC sensor. The palladium implantation was done at 500 C into the Si face of 6H, N-type SiC at various energies, and at various fluences. Then, we measured the hydrogen sensitivity response of each fabricated sensor by exposing them to hydrogen while monitoring the current flow across the p-n junction(s), with respect to time. The sensitivity of each sensor was measured at temperatures between 27 and 300 C. The response of the SiC sensors produced by Pd implantation has revealed a completely different behaviour than the SiC sensors produced by Pd deposition. In the Pd-deposited SiC sensors as well as in the ones reported in the literature, the current rises in the presence of hydrogen at room temperature as well as at elevated temperatures. In the case of Pd-implanted SiC sensors, the current decreases in the presence of hydrogen whenever the temperature is raised above 100 C. We will present the details and conclusions from the results obtained during this meeting.

Muntele, C. I.↗

NASA NTRS2004

AIN-Based Packaging for SiC High-Temperature Electronics

Packaging made primarily of aluminum nitride has been developed to enclose silicon carbide-based integrated circuits (ICs), including circuits containing SiC-based power diodes, that are capable of operation under conditions more severe than can be withstood by silicon-based integrated circuits. A major objective of this development was to enable packaged SiC electronic circuits to operate continuously at temperatures up to 500 C. AlN-packaged SiC electronic circuits have commercial potential for incorporation into high-power electronic equipment and into sensors that must withstand high temperatures and/or high pressures in diverse applications that include exploration in outer space, well logging, and monitoring of nuclear power systems. This packaging embodies concepts drawn from flip-chip packaging of silicon-based integrated circuits. One or more SiC-based circuit chips are mounted on an aluminum nitride package substrate or sandwiched between two such substrates. Intimate electrical connections between metal conductors on the chip(s) and the metal conductors on external circuits are made by direct bonding to interconnections on the package substrate(s) and/or by use of holes through the package substrate(s). This approach eliminates the need for wire bonds, which have been the most vulnerable links in conventional electronic circuitry in hostile environments. Moreover, the elimination of wire bonds makes it possible to pack chips more densely than was previously possible.

Savrun, Ender↗

NASA NTRS1994

Modeling of stress/strain behavior of fiber-reinforced ceramic matrix composites including stress redistribution

A computational simulation procedure is presented for nonlinear analyses which incorporates microstress redistribution due to progressive fracture in ceramic matrix composites. This procedure facilitates an accurate simulation of the stress-strain behavior of ceramic matrix composites up to failure. The nonlinearity in the material behavior is accounted for at the constituent (fiber/matrix/interphase) level. This computational procedure is a part of recent upgrades to CEMCAN (Ceramic Matrix Composite Analyzer) computer code. The fiber substructuring technique in CEMCAN is used to monitor the damage initiation and progression as the load increases. The room-temperature tensile stress-strain curves for SiC fiber reinforced reaction-bonded silicon nitride (RBSN) matrix unidirectional and angle-ply laminates are simulated and compared with experimentally observed stress-strain behavior. Comparison between the predicted stress/strain behavior and experimental stress/strain curves is good. Collectively the results demonstrate that CEMCAN computer code provides the user with an effective computational tool to simulate the behavior of ceramic matrix composites.

Mital, Subodh K.↗

NASA NTRS2000

Durability Evaluation of a Thin Film Sensor System With Enhanced Lead Wire Attachments on SiC/SiC Ceramic Matrix Composites

An advanced thin film sensor system instrumented on silicon carbide (SiC) fiber reinforced SiC matrix ceramic matrix composites (SiC/SiC CMCs), was evaluated in a Mach 0.3 burner rig in order to determine its durability to monitor material/component surface temperature in harsh environments. The sensor system included thermocouples in a thin film form (5 microns thick), fine lead wires (75 microns diameter), and the bonds between these wires and the thin films. Other critical components of the overall system were the heavy, swaged lead wire cable (500 microns diameter) that contained the fine lead wires and was connected to the temperature readout, and ceramic attachments which were bonded onto the CMCs for the purpose of securing the lead wire cables, The newly developed ceramic attachment features a combination of hoops made of monolithic SiC or SiC/SiC CMC (which are joined to the test article) and high temperature ceramic cement. Two instrumented CMC panels were tested in a burner rig for a total of 40 cycles to 1150 C (2100 F). A cycle consisted of rapid heating to 1150 C (2100 F), a 5 minute hold at 1150 C (2100 F), and then cooling down to room temperature in 2 minutes. The thin film sensor systems provided repeatable temperature measurements for a maximum of 25 thermal cycles. Two of the monolithic SiC hoops debonded during the sensor fabrication process and two of the SiC/SiC CMC hoops failed during testing. The hoops filled with ceramic cement, however, showed no sign of detachment after 40 thermal cycle test. The primary failure mechanism of this sensor system was the loss of the fine lead wire-to-thin film connection, which either due to detachment of the fine lead wires from the thin film thermocouples or breakage of the fine wire.

Lei, Jih-Fen↗

NASA NTRS2002

C-Coupon Studies of SiC/SiC Composites: Acoustic Emission Monitoring - Part 1

Modal acoustic emission (AE) was used to monitor the acoustic activity during room temperature and elevated temperature c-coupon tests for a variety of SiC/SiC systems including composites containing Sylramic (trademark), ZMI (trademark), or Hi-Nicalon (trademark) fibers with melt-infiltrated or polymer-infiltrated SiC matrices. Modal AE proved excellent at monitoring matrix cracking in the curved portion of the C-coupon specimen with increasing load. This included the load at which the first AE event occurred and the location of AE events during the test that were, presumably, caused by the formation and growth of interlaminar cracks and, at higher loads, transverse cracks. Graphical techniques were employed to estimate the load for first AE. It was determined that for this test with these material systems, the first AE could be estimated within the load range bounded by the load at which initial deviation from linearity of the load-displacement curve occurs and the load where the 98% offset of the linear regression fit intercepted the load-displacement curve. The calculation of interlaminar tensile (ILT) stress from the load for first AE was determined for all the systems. Ultimate ILT strength usually corresponded to ILT stress determined from the ultimate load to failure of the C-coupon test, which was considerably higher than the first cracking stress.

Morscher, Gregory N.↗

NASA NTRS2011

Development of an Extreme High Temperature n-type Ohmic Contact to Silicon Carbide

We report on the initial demonstration of a tungsten-nickel (75:25 at. %) ohmic contact to silicon carbide (SiC) that performed for up to fifteen hours of heat treatment in argon at 1000 C. The transfer length method (TLM) test structure was used to evaluate the contacts. Samples showed consistent ohmic behavior with specific contact resistance values averaging 5 x 10-4 -cm2. The development of this contact metallization should allow silicon carbide devices to operate more reliably at the present maximum operating temperature of 600 C while potentially extending operations to 1000 C. Introduction Silicon Carbide (SiC) is widely recognized as one of the materials of choice for high temperature, harsh environment sensors and electronics due to its ability to survive and continue normal operation in such environments [1]. Sensors and electronics in SiC have been developed that are capable of operating at temperatures of 600 oC. However operating these devices at the upper reliability temperature threshold increases the potential for early degradation. Therefore, it is important to raise the reliability temperature ceiling higher, which would assure increased device reliability when operated at nominal temperature. There are also instances that require devices to operate and survive for prolonged periods of time above 600 oC [2, 3]. This is specifically needed in the area of hypersonic flight where robust sensors are needed to monitor vehicle performance at temperature greater than 1000 C, as well as for use in the thermomechanical characterization of high temperature materials (e.g. ceramic matrix composites). While SiC alone can withstand these temperatures, a major challenge is to develop reliable electrical contacts to the device itself in order to facilitate signal extraction

Evans, Laura J.↗

NASA NTRS2003

Matrix Cracking in Four Different 2D SiC/SiC Composite Systems

Silicon carbide fiber reinforced, silicon carbide matrix composites are some of the most advanced composite systems for high-temperature, high-stress applications in oxidizing environments. A basic area that needs to be understood for the purpose of material behavior modeling and optimization is the architectural, constituent, and mechanistic factors that contribute to non-linear stress-strain behavior. The mechanism that causes non-linear stress-strain in dense-matrix composites is the formation and propagation of bridged matrix cracks. In addition, the occurrence and propagation of matrix cracks controls the time-dependent strength-properties of these materials in oxidizing environments at elevated temperatures. A modal acoustic emission technique has been used to monitor and estimate the stress-dependent matrix cracking. Two different SiC matrix systems, chemical vapor infiltrated (CVI) and melt-infiltrated (MI), with two different SiC fiber reinforcement, Hi-Nicalon (trademark) and Sylramic (trademark) were compared. Even though the averages of the range where matrix cracking occurred for the composites varied by more than 0.1% in strain and almost 200 MPa in stress, the range or distribution for matrix cracking could be reduced to a narrow band of stress for CVI SiC and MI SiC composites if it were assumed that all matrix cracks emanate outside of the load-bearing fiber, interphase, CVI preform minicomposite. A simple relationship was determined to describe stress-dependent matrix cracking which can then be used to estimate the onset of large, bridged matrix cracks or for material behavior models.

Morscher, Gregory N.↗

NASA NTRS2004

NASA Tech Briefs, March 2004

Topics covered include: 1) Advanced Signal Conditioners for Data-Acquisition Systems; 2) Downlink Data Multiplexer; 3) Viewing ISS Data in Real Time via the Internet; 4) Autonomous Environment-Monitoring Networks; 5) Readout of DSN Monitor Data; 6) Parallel-Processing Equalizers for Multi-Gbps Communications; 7) AIN-Based Packaging for SiC High-Temperature Electronics; 8) Software for Optimizing Quality Assurance of Other Software; 9) The TechSat 21 Autonomous Sciencecraft Experiment; 10) Software for Analyzing Laminar-to-Turbulent Flow Transitions; 11) Elastomer Filled With Single-Wall Carbon Nanotubes; 12) Modifying Ship Air-Wake Vortices for Aircraft Operations; 13) Strain-Gauge Measurement of Weight of Fluid in a Tank; 14) Advanced Docking System With Magnetic Initial Capture; 15) Blade-Pitch Control for Quieting Tilt-Rotor Aircraft; 16) Solar Array Panels With Dust-Removal Capability; 17) Aligning Arrays of Lenses and Single-Mode Optical Fibers; 18) Automatic Control of Arc Process for Making Carbon Nanotubes; 19) Curved-Focal-Plane Arrays Using Deformed-Membrane Photodetectors; 20) Role of Meteorology in Flights of a Solar-Powered Airplane; 21) Model of Mixing Layer With Multicomponent Evaporating Drops; 22) Solution-Assisted Optical Contacting; 23) Improved Discrete Approximation of Laplacian of Gaussian; 24) Utilizing Expert Knowledge in Estimating Future STS Costs; 25) Study of Rapid-Regression Liquefying Hybrid Rocket Fuels; and 26) More About the Phase-Synchronized Enhancement Method.

Source record↗

NASA NTRS2011

NASA Tech Briefs, May 2011

Topics covered include: 1) Method to Estimate the Dissolved Air Content in Hydraulic Fluid; 2) Method for Measuring Collimator-Pointing Sensitivity to Temperature Changes; 3) High-Temperature Thermometer Using Cr-Doped GdAlO3 Broadband Luminescence; 4)Metrology Arrangement for Measuring the Positions of Mirrors of a Submillimeter Telescope; 5) On-Wafer S-Parameter Measurements in the 325-508-GHz Band; 6) Reconfigurable Microwave Phase Delay Element for Frequency Reference and Phase-Shifter Applications; 7) High-Speed Isolation Board for Flight Hardware Testing; 8) High-Throughput, Adaptive FFT Architecture for FPGA-Based Spaceborne Data Processors; 9) 3D Orbit Visualization for Earth-Observing Missions; 10) MaROS: Web Visualization of Mars Orbiting and Landed Assets; 11) RAPID: Collaborative Commanding and Monitoring of Lunar Assets; 12) Image Segmentation, Registration, Compression, and Matching; 13) Image Calibration; 14) Rapid ISS Power Availability Simulator; 15) A Method of Strengthening Composite/Metal Joints; 16) Pre-Finishing of SiC for Optical Applications; 17) Optimization of Indium Bump Morphology for Improved Flip Chip Devices; 18) Measuring Moisture Levels in Graphite Epoxy Composite Sandwich Structures; 19) Marshall Convergent Spray Formulation Improvement for High Temperatures; 20) Real-Time Deposition Monitor for Ultrathin Conductive Films; 21) Optimized Li-Ion Electrolytes Containing Triphenyl Phosphate as a Flame-Retardant Additive; 22) Radiation-Resistant Hybrid Lotus Effect for Achieving Photoelectrocatalytic Self-Cleaning Anticontamination Coatings; 23) Improved, Low-Stress Economical Submerged Pipeline; 24) Optical Fiber Array Assemblies for Space Flight on the Lunar Reconnaissance Orbiter; 25) Local Leak Detection and Health Monitoring of Pressurized Tanks; 26) Dielectric Covered Planar Antennas at Submillimeter Wavelengths for Terahertz Imaging; 27) Automated Cryocooler Monitor and Control System; 28) Broadband Achromatic Phase Shifter for a Nulling Interferometer; 29) Super Dwarf Wheat for Growth in Confined Spaces; 30) Fine Guidance Sensing for Coronagraphic Observatories; 31) Single-Antenna Temperature- and Humidity-Sounding Microwave Receiver; 32) Multi-Wavelength, Multi-Beam, and Polarization-Sensitive Laser Transmitter for Surface Mapping; 33) Optical Communications Link to Airborne Transceiver; 34) Ascent Heating Thermal Analysis on Spacecraft Adaptor Fairings; 35) Entanglement in Self-Supervised Dynamics; 36) Prioritized LT Codes; 37) Fast Image Texture Classification Using Decision Trees; 38) Constraint Embedding Technique for Multibody System Dynamics; 39) Improved Systematic Pointing Error Model for the DSN Antennas; 40) Observability and Estimation of Distributed Space Systems via Local Information-Exchange Networks; 41) More-Accurate Model of Flows in Rocket Injectors; 42) In-Orbit Instrument-Pointing Calibration Using the Moon as a Target; 43) Reliability of Ceramic Column Grid Array Interconnect Packages Under Extreme Temperatures; 44) Six Degrees-of-Freedom Ascent Control for Small-Body Touch and Go; and 45) Optical-Path-Difference Linear Mechanism for the Panchromatic Fourier Transform Spectrometer.

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NASA NTRS2005

Damage Accumulation in SiC/SiC Composites with 3D Architecture

Matrix cracking in Sic fiber reinforced, melt-infiltrated Sic composites with 3D orthogonal architectures was determined for specimens tested in tension at room temperature. Acoustic emission (AE) was used to monitor the matrix cracking activity and was later confirmed by microscopic examination of specimens that had failed. Exact location of AE demonstrated that initial cracking occurred in the matrix rich regions when a large z-direction fiber bundle was used. For specimens with large z-direction fiber tows, the earliest matrix cracking could occur at half the stress for standard 2D woven composites with similar constituents.

Yun, Hee-Mann↗

NASA NTRS2011

Detecting Damage in Ceramic Matrix Composites Using Electrical Resistance

The majority of damage in SiC/SiC ceramic matrix composites subjected to monotonic tensile loads is in the form of distributed matrix cracks. These cracks initiate near stress concentrations, such as 90 deg fiber tows or large matrix pores and continue to accumulate with additional stress until matrix crack saturation is achieved. Such damage is difficult to detect with conventional nondestructive evaluation techniques (immersion ultrasonics, x-ray, etc.). Monitoring a specimen.s electrical resistance change provides an indirect approach for monitoring matrix crack density. Sylramic-iBN fiber- reinforced SiC composites with a melt infiltrated (MI) matrix were tensile tested at room temperature. Results showed an increase in resistance of more than 500% prior to fracture, which can be detected either in situ or post-damage. A relationship between resistance change and matrix crack density was also determined.

Smith, Craig E.↗

NASA NTRS2011

Detecting Cracks in Ceramic Matrix Composites by Electrical Resistance

The majority of damage in SiC/SiC ceramic matrix composites subjected to monotonic tensile loads is in the form of distributed matrix cracks. These cracks initiate near stress concentrations, such as 90o fiber tows or large matrix pores and continue to accumulate with additional stress until matrix crack saturation is achieved. Such damage is difficult to detect with conventional nondestructive evaluation techniques (immersion ultrasonics, x-ray, etc.). Monitoring a specimen.s electrical resistance change provides an indirect approach for monitoring matrix crack density. Sylramic-iBN fiber- reinforced SiC composites with a melt infiltrated (MI) matrix were tensile tested at room temperature. Results showed an increase in resistance of more than 500% prior to fracture, which can be detected either in situ or post-damage. A relationship between resistance change and matrix crack density was also determined.

Smith, Craig↗

NASA NTRS2001

Room Temperature Creep Of SiC/SiC Composites

During a recent experimental study, time dependent deformation was observed for a damaged Hi-Nicalon reinforced, BN interphase, chemically vapor infiltrated SiC matrix composites subjected to static loading at room temperature. The static load curves resembled primary creep curves. In addition, acoustic emission was monitored during the test and significant AE activity was recorded while maintaining a constant load, which suggested matrix cracking or interfacial sliding. For similar composites with carbon interphases, little or no time dependent deformation was observed. Evidently, exposure of the BN interphase to the ambient environment resulted in a reduction in the interfacial mechanical properties, i.e. interfacial shear strength and/or debond energy. These results were in qualitative agreement with observations made by Eldridge of a reduction in interfacial shear stress with time at room temperature as measured by fiber push-in experiments.

Morscher, Gregory N.↗

NASA NTRS2003

Damage Accumulation in SiC/SiC Composites with 3D Architectures

The formation and propagation of multiple matrix cracks in relatively dense ceramic matrix composites when subjected to increasing tensile stress is necessary for high strength and tough composites. However, the occurrence of matrix cracks at low stresses may limit the usefulness of some non-oxide composite systems when subjected to oxidizing environments for long times at stresses sufficient to cause matrix cracking. For SiC fiber-reinforced composites with two-dimensional woven architectures and chemically vapor infiltrated (CVI) SiC matrix and melt-infiltrated (MI) Si/SiC matrix composites, the matrix cracking behavior has been fairly well characterized for different fiber-types and woven architectures. It was found that the occurrence, degree, and growth of matrix cracks depends on the material properties of the composite constituents as well as other physical properties of the composite or architecture, e.g., matrix porosity and size of the fiber bundle. In this study, matrix cracking in SiC fiber reinforced, melt-infiltrated SiC composites with a 3D orthogonal architecture was determined for specimens tested in tension at room temperature. Acoustic emission (AE) was used to monitor the matrix cracking activity, which was later confirmed by microscopic examination of specimens that had failed. The determination of the exact location of AE demonstrated that initial cracking occurred in the matrix rich regions when a large z-direction fiber bundle was used. For specimens with large z-direction fiber tows, the earliest matrix cracking could occur at half the stress for standard 2D woven composites with similar constituents. Damage accumulation in 3D architecture composites will be compared to damage accumulation in 2D architecture composites and discussed with respect to modeling composite stress-strain behavior and use of these composites at elevated temperatures.

Morscher, Gregory N.↗