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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.↗

NASA NTRS1998

Room Temperature Tensile Behavior and Damage Accumulation of Hi-Nicalon Reinforced SiC Matrix Composites

Composites consisting of woven Hi-Nicalon fibers, BN interphases, and different SiC matrices were studied in tension at room temperature. Composites with SiC matrices processed by CVI and melt infiltration were compared. Monotonic and load/unload/reload tensile hysteresis experiments were performed. A modal acoustic emission (AE) analyzer was used to monitor damage accumulation during the tensile test. Post test polishing of the tensile gage sections was performed to determine the extent of cracking. The occurrence and location of cracking could easily be determined using modal AE. The loss of modulus could also effectively be determined from the change in the velocity of sound across the sample. Finally, the stresses where cracks appear to intersect the load-bearing fibers correspond with high temperature low cycle fatigue run out stresses for these materials.

Morscher, G. N.↗

NASA NTRS2000

Intermediate Temperature Stress Rupture of Woven SiC Fiber, BN Interphase, SiC Matrix Composites in Air

Tensile stress-rupture experiments were performed on woven Hi-Nicalon reinforced SiC matrix composites with BN interphases in air. Modal acoustic emission (AE) was used to monitor the damage accumulation in the composites during the tests and microstructural analysis was performed to determine the amount of matrix cracking that occurred for each sample. Fiber fractograph), was also performed for individual fiber failures at the specimen fracture surface to determine the strengths at which fibers failed. The rupture strengths were significantly worse than what would have been expected front the inherent degradation of the fibers themselves when subjected to similar rupture conditions. At higher applied stresses the rate of rupture "?as larger than at lower applied stresses. It was observed that the change in rupture rate corresponded to the onset of through-thickness cracking in the composites themselves. The primary cause of the sen,ere degradation was the ease with which fibers would bond to one another at their closest separation distances, less than 100 nanometers, when exposed to the environment. The near fiber-to-fiber contact in the woven tows enabled premature fiber failure over large areas of matrix cracks due to the stress-concentrations created b), fibers bonded to one another after one or a few fibers fail. i.e. the loss of global load sharing. An@, improvement in fiber-to-fiber separation of this composite system should result in improved stress- rupture properties. A model was den,eloped in order to predict the rupture life-time for these composites based on the probabilistic nature of indin,idual fiber failure at temperature. the matrix cracking state during the rupture test, and the rate of oxidation into a matrix crack. Also incorporated into the model were estimates of the stress-concentration that would occur between the outer rim of fibers in a load-bearing bundle and the unbridged region of a matrix crack after Xia et al. For the lower stresses, this source of stress-concentration was the likely cause for initial fiber failure that would trigger catastrophic failure of the composite.

Morscher, Gregory N.↗

NASA NTRS2000

Room and Elevated Temperature Tensile Properties of Single Tow Hi-Nicalon, Carbon Interphase, CVI SiC Matrix Minicomposites

Single tow Hi-Nicalon(TM), C interphase, CVI SiC matrix minicomposites were tested in tension at room temperature, 700 C, 950 C, and 1200 C in air. Monotonic loading with modal acoustic emission monitoring was performed at room temperature in order to determine the dependence of matrix cracking on applied load. Modal acoustic emission was shown to correlate directly with the number of matrix cracks formed. Elevated temperature constant load stress-rupture and low-cycle fatigue experiments were performed on precracked specimens. The elevated temperature rupture behavior was dependent on the precrack stress, the lower precrack stress resulting in longer rupture life for a given stress. It was found that the rupture lives of C-interphase Hi-Nicalon(TM) minicomposites were superior to C-interphase Ceramic Grade Nicalon(TM) minicomposites and inferior to those of BN-interphase Hi-Nicalon(TM) minicomposites.

Martinez-Fernandez, J.↗

NASA NTRS2002

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

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

Zhu, Dongming↗

NASA NTRSDate not supplied

Pt/HTCC Alumina based Electronic Packaging System and Integration Processes for High Temperature Harsh Environment Applications

Electronic devices capable of operation at 500°C are required for long term Venus surface missions, as well as for in situ monitoring and control of next generation aeronautical engines. High temperature sensors and electronics can also find many applications in military, and energy and automobile industries. Various silicon carbide (SiC) sensors and electronic devices have been developed for operation at 500 °C, and a compatible packaging system is needed for long term test and deployment of these high temperature devices. High temperature co-fired ceramics (HTCC) alumina with platinum (Pt) conductor was proposed for high temperature electronic packaging. A prototype Pt/HTCC alumina packaging system including chip-level package and circuit board has been briefly reported previously for long-term electrical testing of SiC integrated circuits at 500 °C, and brief testing at much higher temperatures. HTCC alumina is an excellent dielectric material with acceptable dielectric constant and low dielectric loss over wide temperature and frequency ranges. Pt is chemically noble and can be co-fired with HTCC alumina in air ambient producing a viable electronic packaging material system for high temperature applications. This paper presents a more detailed description of this packaging system including prototype low power packages and circuit boards based on HTCC alumina and Pt metallization for 500°C and other harsh environment applications. The key technical considerations for chip-level packaging and circuit board assembly, including materials and processes for 500 °C durable wire-bonding and SiC die attach, and integration of multi-chip circuit boards, are presented. Experimental test results of this packaging approach applied to SiC integrated circuits at 500 °C and 700°C are discussed as well.

High temperature↗

NASA NTRSDate not supplied

Pt/HTCC Alumina based Electronic Packaging System and Integration Processes for High Temperature Harsh Environment Applications

electronic packaging↗

NASA NTRS2001

Characterization and In-Situ Monitoring of ZnSe Crystal Growth by Seeded PVT for Microgravity Applications

Crystal growth from the vapor phase continues to play a significant role in the production of II-VI semiconductor compounds (ZnO, ZnTe, CdTe, etc.) and SiC. As compared to melt growth methods (where available) the advantages are: (1) lower growth temperature(s); (2) reduction in defect concentration; (3) additional purification; and (4) enhanced crystal perfection. A powerful tool in determining the mechanism of PVT is microgravity. Under normal gravity conditions the transport mechanism is a superposition of diffusive and convective fluxes. Microgravity offers the possibility of studying the transport properties without the influence of convective effects. Research on the crystal growth of ZnSe by PVT (P.I.: Su of NASA/MSFC) will help to clarify the effects of convection on crystal growth. A crystal growth furnace with in-situ and real time optical monitoring capabilities was constructed and used to monitor the vapor composition and growing crystal surface morphology during the PVT growth of ZnSe. Using photoluminescence and SIMS, ex-situ, the incorporation of point defects (Zn vacancy) and impurities was found to be correlated to the gravity vector due to the influence of the convective flow. A summary of the results to date will be presented.

Feth, Shari T.↗

NASA NTRS2001

Stress-Rupture and Stress-Relaxation of SiC/SiC Composites at Intermediate Temperature

Tensile static stress and static strain experiments were performed on woven Sylramic (Dow Corning, Midland, MI) and Hi-Nicalon (Nippon Carbon, Japan) fiber reinforced, BN interphase, melt-infiltrated SiC matrix composites at 815 C. Acoustic emission was used to monitor the damage accumulation during the test. The stress-rupture properties of Sylramic composites were superior to that of Hi-Nicalon Tm composites. Conversely, the applied strain levels that Hi-Nicalon composites can withstand for stress-relaxation experiments were superior to Sylramic composites; however, at a cost of poor retained strength properties for Hi-Nicalon composites. Sylramic composites exhibited much less stress-oxidation induced matrix cracking compared to Hi-Nicalon composites. This was attributed to the greater stiffness and roughness of Sylramic fibers themselves and the lack of a carbon layer between the fiber and the BN interphase for Sylramic composites, which existed in Hi-Nicalon composites. Due to the lack of stress-relief for Sylramic composites, time to failure for Sylramic composite stress-relaxation experiments was not much longer than for stress-rupture experiments when comparing the peak stress condition for stress-relaxation with the applied stress of stress-rupture.

Morscher, Gregory N.↗

NASA NTRS1988

Dynamic fracture toughness of ceramic composites

The dynamic fracture toughness vs crack velocity relationships of TiB2 particulate-reinforced SiC-matrix and SiC whisker-reinforced Al2O3-matrix composites were determined at both room temperature and 1200 C with impacted, single-edge notched three-point bend specimens. Rapid crack initiation and propagation were monitored by a laser interferometric-displacement gage system. A FEM model that transmitted the measured outside-impact load to the specimen within the furnace was used to characterize the entire loading system-specimen unit. Small differences were measured between the room temperature and 1200 C dynamic responses.

Yang, K. H.↗

NASA NTRS1998

The Evolution of Interfacial Sliding Stresses During Cyclic Push-in Testing of C- and BN-Coated Hi-Nicalon Fiber-Reinforced CMCs

Interfacial debond cracks and fiber/matrix sliding stresses in ceramic matrix composites (CMCs) can evolve under cyclic fatigue conditions as well as with changes in the environment, strongly affecting the crack growth behavior, and therefore, the useful service lifetime of the composite. In this study, room temperature cyclic fiber push-in testing was applied to monitor the evolution of frictional sliding stresses and fiber sliding distances with continued cycling in both C- and BN-coated Hi-Nicalon SiC fiber-reinforced CMCs. A SiC matrix composite reinforced with C-coated Hi-Nical on fibers as well as barium strontium aluminosilicate (BSAS) matrix composites reinforced with BN-coated (four different deposition processes compared) Hi-Nicalon fibers were examined. For failure at a C interface, test results indicated progressive increases in fiber sliding distances during cycling in room air but not in nitrogen. These results suggest the presence of moisture will promote crack growth when interfacial failure occurs at a C interface. While short-term testing environmental effects were not apparent for failure at the BN interfaces, long-term exposure of partially debonded BN-coated fibers to humid air resulted in large increases in fiber sliding distances and decreases in interfacial sliding stresses for all the BN coatings, presumably due to moisture attack. A wide variation was observed in debond and frictional sliding stresses among the different BN coatings.

Eldridge, J. I.↗

NASA NTRS2002

Acoustic Emission and Damage Accumulation for Various Woven C/SiC Composites Tested in Tension at Room Temperature

Modal acoustic emission (AE) has proven to be an excellent technique to monitor damage accumulation in ceramic matrix composites. In this study, AE was used to monitor tensile load-unload-reload hysteresis tests for a variety of C fiber reinforced, SiC matrix composites. C/SiC composites were reinforced with T300 and IM7 fibers, had C, multilayer, or pseudo-porous C interphases, and had chemical vapor infiltrated SiC or melt-infiltrated SiC matrices. All of the composites exhibited considerable AE during testing. The extent and nature of the AE activity will be analyzed and discussed in light of matrix cracking and the variety of composite constituents. It is hoped that understanding the nature of stress dependent damage accumulation in these materials can be of use in life modeling for these types of composites.

Morscher, Gregory N.↗

NASA NTRS2002

Acoustic Emission and Damage Accumulation for Various Woven C/SiC Composites Tested in Tension at Room Temperature

Modal acoustic emission (AE) has proven to be an excellent technique to monitor damage accumulation in ceramic matrix composites. In this study, AE was used to monitor tensile load-unload-reload hysteresis tests for a variety of C fiber reinforced, Sic matrix composites. C/SiC composites were reinforced with T-300 and IM7 fibers, had C, multilayer, or pseudo-porous C interphases, and had chemical vapor infiltrated Sic or melt-infiltrated SiC matrices. All of the composites exhibited considerable AE during testing. The extent and nature of the AE activity will be analyzed and discussed in light of matrix cracking and the variety of composite constituents. It is hoped that understanding the nature of stress-dependent damage accumulation in these materials can be of use in life-modeling for these types of composites.

Morscher, Gregory↗

NASA NTRS1999

Intermediate Temperature Stress Rupture of a Woven Hi-Nicalon, BN-Interphase, SiC Matric Composite in Air

Woven Hi-Nicalon (TM) reinforced melt-infiltrated SiC matrix composites were tested under tensile stress-rupture conditions in air at intermediate temperatures. A comprehensive examination of the damage state and the fiber properties at failure was performed. Modal acoustic emission analysis was used to monitor damage during the experiment. Extensive microscopy of the composite fracture surfaces and the individual fiber fracture surfaces was used to determine the mechanisms leading to ultimate failure. The rupture properties of these composites were significantly worse than expected compared to the fiber properties under similar conditions. This was due to the oxidation of the BN interphase. Oxidation occurred through the matrix cracks that intersected the surface or edge of a tensile bar. These oxidation reactions resulted in minor degradation to fiber strength and strong bonding of the fibers to one another at regions of near fiber-to-fiber contact. It was found that two regimes for rupture exist for this material: a high stress regime where rupture occurs at a fast rate and a low stress regime where rupture occurs at a slower rate. For the high stress regime, the matrix damage state consisted of through thickness cracks. The average fracture strength of fibers that were pulled-out (the final fibers to break before ultimate failure) was controlled by the slow-crack growth rupture criterion in the literature for individual Hi-Nicalon (TM) fibers. For the low stress regime, the matrix damage state consisted of microcracks which grew during the rupture test. The average fracture strength of fibers that were pulled-out in this regime was the same as the average fracture strength of individual fibers pulled out in as-produced composites tested at room temperature.

Morscher, Gregory N.↗

NASA NTRS2005

Pd/CeO2/SiC Chemical Sensors

The incorporation of nanostructured interfacial layers of CeO2 has been proposed to enhance the performances of Pd/SiC Schottky diodes used to sense hydrogen and hydrocarbons at high temperatures. If successful, this development could prove beneficial in numerous applications in which there are requirements to sense hydrogen and hydrocarbons at high temperatures: examples include monitoring of exhaust gases from engines and detecting fires. Sensitivity and thermal stability are major considerations affecting the development of high-temperature chemical sensors. In the case of a metal/SiC Schottky diode for a number of metals, the SiC becomes more chemically active in the presence of the thin metal film on the SiC surface at high temperature. This increase in chemical reactivity causes changes in chemical composition and structure of the metal/SiC interface. The practical effect of the changes is to alter the electronic and other properties of the device in such a manner as to degrade its performance as a chemical sensor. To delay or prevent these changes, it is necessary to limit operation to a temperature <450 C for these sensor structures. The present proposal to incorporate interfacial CeO2 films is based partly on the observation that nanostructured materials in general have potentially useful electrical properties, including an ability to enhance the transfer of electrons. In particular, nanostructured CeO2, that is CeO2 with nanosized grains, has shown promise for incorporation into hightemperature electronic devices. Nanostructured CeO2 films can be formed on SiC and have been shown to exhibit high thermal stability on SiC, characterized by the ability to withstand temperatures somewhat greater than 700 C for limited times. The exchanges of oxygen between CeO2 and SiC prevent the formation of carbon and other chemical species that are unfavorable for operation of a SiC-based Schottky diode as a chemical sensor. Consequently, it is anticipated that in a Pd/CeO2/SiC Schottky diode, the nanostructured interfacial CeO2 layer would contribute to thermal stability and, by contributing to transfer of electrons, would also contribute to sensitivity.

Lu, Weijie↗

NASA NTRS2004

Effect of Specimen Thickness on Mechanical Behavior of SiC/SiC Composites

Potential composite applications in aerospace and transportation application systems have different thickness requirements. For example, space applications such as nozzle ramps or heat exchangers use very thin (less than 1 mm) structures whereas turbine blades need very thick parts greater than or equal to cm). There has been little investigation into the effect of thickness on stress-strain behavior or elevated temperature tensile properties controlled by oxidation. In this study, composites consisting of woven Hi-NicalonTM fibers, a carbon interphase, and CVI Sic matrix were fabricated with different numbers of plies to provide variable thickness. The composites ranged from a single ply (approximately 0.4 mm) to thirty-six plies (approximately 1 cm). Tensile tests were performed at room temperature with acoustic emission used to monitor matrix crack behavior. Elevated temperature tensile stress-rupture tests were performed in air. Considerably different room and elevated temperature tensile behavior was observed that will be discussed with respect to the effect of thickness on matrix crack formation, matrix crack growth and oxidation diffusion kinetics.

Morscher, Gregory N.↗

NASA NTRS1992

Damage mechanisms in three-dimensional woven reinforced ceramic matrix composites under tensile and flexural loading at room and elevated temperatures

Three-dimensional Nicalon SiC/SiC matrix composites made through a chemical vapor infiltration process were studied under tensile and flexural loading at 23, 1200, and 1550 C in air. In situ damage accumulation monitoring NDE techniques were utilized to identify failure mechanisms in these materials. The effectiveness and durability of a chemical vapor deposition SiC surface coating were also evaluated in severe oxidizing environment. Results show that the failure response was very similar for the 23 and 1200 C specimens, while at 1550 C there were significant changes in both the composite mechanical behavior and the matrix microstructure. Extensive fiber pull-out was observed only in the 1550 C specimen. It is also found that the SiC surface coating can protect the composite up to the critical matrix cracking strength.

Chulya, Abhisak↗

NASA NTRS2012

Alumina Based 500 C Electronic Packaging Systems and Future Development

NASA space and aeronautical missions for probing the inner solar planets as well as for in situ monitoring and control of next-generation aeronautical engines require high-temperature environment operable sensors and electronics. A 96% aluminum oxide and Au thick-film metallization based packaging system including chip-level packages, printed circuit board, and edge-connector is in development for high temperature SiC electronics. An electronic packaging system based on this material system was successfully tested and demonstrated with SiC electronics at 500 C for over 10,000 hours in laboratory conditions previously. In addition to the tests in laboratory environments, this packaging system has more recently been tested with a SiC junction field effect transistor (JFET) on low earth orbit through the NASA Materials on the International Space Station Experiment 7 (MISSE7). A SiC JFET with a packaging system composed of a 96% alumina chip-level package and an alumina printed circuit board mounted on a data acquisition circuit board was launched as a part of the MISSE7 suite to International Space Station via a Shuttle mission and tested on the orbit for eighteen months. A summary of results of tests in both laboratory and space environments will be presented. The future development of alumina based high temperature packaging using co-fired material systems for improved performance at high temperature and more feasible mass production will also be discussed.

Chen, Liang-Yu↗