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As-received desert sand from a Middle East country has been characterized for its phase composition and thermal stability. X-ray diffraction analysis showed the presence of quartz (SiO2), calcite (CaCO3), gypsum (CaSO4.2H2O), and NaAlSi3O8 phases in as-received desert sand and showed weight loss of approx. 35 percent due to decomposition of CaCO3 and CaSO4.2H2O when heated to 1400 C. A batch of as-received desert sand was melted into calcium magnesium aluminosilicate (CMAS) glass at approx. 1500 C. From inductively coupled plasma-atomic emission spectrometry, chemical composition of the CMAS glass was analyzed to be 27.8CaO-4MgO-5Al2O3-61.6SiO2-0.6Fe2O3-1K2O (mole percent). Various physical, thermal and mechanical properties of the glass have been evaluated. Bulk density of CMAS glass was 2.69 g/cc, Young's modulus 92 GPa, Shear modulus 36 GPa, Poisson's ratio 0.28, dilatometric glass transition temperature (T (sub g)) 706 C, softening point (T (sub d)) 764 C, Vickers microhardness 6.3 +/- 0.4 GPa, indentation fracture toughness 0.75 +/- 0.15 MPa.m (sup 1/2), and coefficient of thermal expansion (CTE) 9.8 x 10 (exp -6)/degC in the temperature range 25 to 700 C. Temperature dependence of viscosity has also been estimated from various reference points of the CMAS glass using the Vogel-Fulcher-Tamman (VFT) equation. The glass remained amorphous after heat treating at 850 C for 10 hr but crystallized into CaSiO3 and Ca-Mg-Al silicate phases at 900 C or higher temperatures. Crystallization kinetics of the CMAS glass has also been investigated by differential thermal analysis (DTA). Activation energies for the crystallization of two different phases in the glass were calculated to be 403 and 483 kJ/mol, respectively.

The combined mode I-mode II fracture behavior of anisotropic ZrO2-8wt%Y2O3 thermal barrier coatings was determined in asymmetric flexure loading at both ambient and elevated temperatures. A fracture envelope of KI versus KII was determined for the coating material at ambient and elevated temperatures. Propagation angles of fracture as a function of KI/KII were also determined. The mixed-mode fracture behavior of the microsplat coating material was modeled using Finite Element approach to account for anisotropy and micro cracked structures, and predicted in terms of fracture envelope and propagation angle using mixed-mode fracture theories.

Impact performance of 2-D woven SiC/SiC composites coated with 225 and 525 m thick environmental barrier coating (EBC) was investigated. The composites were fabricated by melt infiltration and the EBC was deposited by plasma spray. Impact tests were conducted at room temperature and at 1316 C in air using 1.59-mm diameter steel-balls at projectile velocities ranging from 110 to 375 m/s. Both microscopy and nondestructive evaluation (NDE) methods were used to determine the extent of damage in the substrate and coating with increasing projectile velocity. The impacted specimens were tensile tested at room temperature to determine their residual mechanical properties. At projectile velocities less than 125 m/s, no detectable damage was noticed in the MI SiC/SiC composites coated with 525 m EBC. With increase in projectile velocity beyond this value, spallation of EBC layers, delamination of fiber plies, and fiber fracture were detected. At a fixed projectile velocity, the composites coated with 525 m EBC showed less damage than the composite coated with 225 m EBC. Both types of EBC coated composites retained a large fraction of the baseline properties of as-fabricated composites and exhibited non-brittle failure after impact testing at projectile velocities up to 375 m/s. Exposure of impact tested specimens in a moisture environment at 1316 C for 500 hr indicated that the through-the-thickness cracks in the EBC coating and delamination cracks in the substrate generated after impact testing acted as conduits for internal oxidation.

Two-dimensional woven SiC/SiC composites fabricated by melt infiltration method were impact tested at room temperature and at 1316 C in air using 1.59-mm diameter steel-ball projectiles at velocities ranging from 115 to 400 m/s. The extent of substrate damage with increasing projectile velocity was imaged and analyzed using optical and scanning electron microscopy, and non-destructive evaluation (NDE) methods such as pulsed thermography, and computed tomography. The impacted specimens were tensile tested at room temperature to determine their residual mechanical properties. Results indicate that at 115 m/s projectile velocity, the composite showed no noticeable surface or internal damage and retained its as-fabricated mechanical properties. As the projectile velocity increased above this value, the internal damage increased and mechanical properties degraded: At velocities >300 m/s, the projectile penetrated through the composite, but the composite retained approx.50% of the ultimate tensile strength of the as-fabricated composite and exhibited non-brittle failure. Predominant internal damages are delamination of fiber plies, fiber fracture and matrix shearing.

Impact performance of 2D woven SiC/SiC composites coated with 225 and 525 microns thick environmental barrier coating (EBC) was investigated. The composites were fabricated by melt infiltration and the EBC was deposited by plasma spray. Impact tests were conducted at room temperature and at 1316 C in air using 1.59 mm diameter steel-balls at projectile velocities ranging from 110 to 375 m/s . Both microscopy and non-destructive evaluation (NDE) methods were used to determine the extent of damage in the substrate and coating with increasing projectile velocity. The impacted specimens were tensile tested at room temperature to determine their residual mechanical properties. At projectile velocities less than 125 m/s , no detectable internal damage was noticed in the MI SiC/SiC composites coated with 525 microns EBC. With increase in projectile velocity beyond this value, spallation of EBC layers, delamination of fiber plies, and fiber fracture were detected. At a fixed projectile velocity, the composites coated with 525 microns EBC showed less damage than those coated with 225 microns EBC. Both types of coated composites retained a large fraction of the baseline properties of the as-fabricated composites and exhibited non-brittle failure after impact testing. Furnace exposure of impacted specimens in a moisture environment at 1316 C for 500 h indicated that the through-the-thickness cracks in the coating and delamination cracks in the substrate generated after impact testing acted as conduits for internal oxidation.

A material consisting of a barium calcium aluminosilicate glass reinforced with 4 weight percent of boron nitride nanotubes (BNNTs) has shown promise for use as a sealant in planar solid oxide fuel cells (SOFCs).

An apparatus for positioning and holding material specimens is a major subsystem of a system for impact testing of the specimens at temperatures up to 1,500 C. This apparatus and the rest of the system are designed especially for hot impact testing of advanced ceramics, composites, and coating materials. The apparatus includes a retaining fixture on a rotating stage on a vertically movable cross support driven by a linear actuator. These components are located below a furnace wherein the hot impact tests are performed (see Figure 1). In preparation for a test, a specimen is mounted on the retaining fixture, then the cross support is moved upward to raise the specimen, through an opening in the bottom of the furnace, to the test position inside the furnace. On one side of the furnace there is another, relatively small opening on a direct line to the specimen. Once the specimen has become heated to the test temperature, the test is performed by using an instrumented external pressurized-gas-driven gun to shoot a projectile through the side opening at the specimen.

Assessments of foreign object damage (FOD) of a commercial, gas-turbine grade, in situ toughened silicon nitride ceramic (AS800, Honeywell Ceramics Components) were made using four different projectile materials at ambient temperature. AS800 flexure target specimens rigidly supported were impacted at their centers in a velocity range from 50 to 450 m/s by spherical projectiles with a diameter of 1.59 mm. Four different projectile materials were used including hardened steel, annealed steel, silicon nitride ceramic, and brass. Post-impact strength of each target specimen impacted was determined as a function of impact velocity to appraise the severity of local impact damage. For a given impact velocity, the degree of strength degradation was greatest for ceramic balls, least for brass balls, and intermediate for annealed and hardened steel balls. For steel balls, hardened projectiles yielded more significant impact damage than annealed counterparts. The most important material parameter affecting FOD was identified as hardness of projectiles. Impact load as a function of impact velocity was quasi-statically estimated based on both impact and static indentation associated data.

Interlaminar shear strength of four different fiber-reinforced ceramic matrix composites was determined with doublenotch shear test specimens as a function of test rate at elevated temperatures ranging from 1100 to 1316 C in air. Life limiting behavior, represented as interlaminar shear strength degradation with decreasing test rate, was significant for 2-D crossplied SiC/MAS-5 and 2-D plain-woven C/SiC composites, but insignificant for 2-D plain-woven SiC/SiC and 2-D woven Sylramic (Dow Corning, Midland, Michigan) SiC/SiC composites. A phenomenological, power-law delayed failure model was proposed to account for and to quantify the rate dependency of interlaminar shear strength of the composites. Additional stress rupture testing in interlaminar shear was conducted at elevated temperatures to validate the proposed model. The model was in good agreement with SiC/MAS-5 and C/SiC composites, but in poor to reasonable agreement with Sylramic SiC/SiC. Constant shear stress-rate testing was proposed as a possible means of life prediction testing methodology for ceramic matrix composites subjected to interlaminar shear at elevated temperatures when short lifetimes are expected.

Fracture toughness of a total of 13 advanced monolithic ceramics including silicon nitrides, silicon carbide, aluminas, and glass ceramic was determined at ambient temperature by using both single edge precracked beam (SEPB) and single edge v-notched beam (SEVNB) methods. Relatively good agreement in fracture toughness between the two methods was observed for advanced ceramics with flat R-curves; whereas, poor agreement in fracture toughness was seen for materials with rising R-curves. The discrepancy in fracture toughness between the two methods was due to stable crack growth with crack closure forces acting in the wake region of cracks even in SEVNB test specimens. The effect of discrepancy in fracture toughness was analyzed in terms of microstructural feature (grain size and shape), toughening exponent in R-curve, and stable crack growth determined using back-face strain gaging.

NASA Glenn Research Center is developing advanced technology for Stirling convertors with a target of significantly improving the specific power and efficiency of the convertor and overall generator for Mars rovers and deep space missions. One specific approach to the target has been recognized as the use of appropriate high-temperature materials. As a series of ceramic material approaches in Advanced Stirling Convertor Development Program in fiscal year 2005, two commercial, structural silicon nitrides AS800 (Honeywell, Torrence, California) and SN282 (Kyocera, Vancouver, Washington) were selected and their mechanical and life limiting properties were characterized at 1050 C in air. AS800 exhibited both strength and Weibull modulus greater than SN282. A life limiting phenomenon was apparent in AS800 with a low slow crack growth parameter n = 15; whereas, a much increased resistance to slow crack growth was found in SN282 with n greater than 100. Difference in elastic modulus and thermal conductivity was negligible up to 1200 C between the two silicon nitrides. The same was true for the coefficient of thermal expansion up to 1400 C.

Solid oxide fuel cell seal glass G18 composites reinforced with approx.4 weight percent of BN nanotubes were fabricated via hot pressing. Room temperature strength and fracture toughness of the composite were determined by four-point flexure and single edge V-notch beam methods, respectively. The strength and fracture toughness of the composite were higher by as much as 90% and 35%, respectively, than those of the glass G18. Microscopic examination of the composite fracture surfaces using SEM and TEM showed pullout of the BN nanotubes, similar in feature to fiber-reinforced ceramic matrix composites with weak interfaces. Other mechanical and physical properties of the composite will also be presented.

Boron nitride nanotubes of significant lengths were synthesized by reaction of boron with nitrogen. Barium calcium aluminosilicate glass composites reinforced with ~4 weight percent of BN nanotubes were fabricated by hot pressing. Ambient-temperature flexure strength and fracture toughness of the glass-BN nanotube composites were determined. The strength and fracture toughness of the composite were higher by as much as 90 and 35 percent, respectively, than those of the unreinforced glass. Microscopic examination of the composite fracture surfaces showed pullout of the BN nanotubes. The preliminary results on the processing and improvement in mechanical properties of BN nanotube reinforced glass matrix composites are being reported here for the first time.

A fuel cell is an electrochemical device that continuously converts the chemical energy of a fuel directly into electrical energy. It consists of an electrolyte, an anode, and a cathode. Various types of fuel cells are available, such as direct methanol fuel cells, alkaline fuel cells, proton-exchange-membrane fuel cells, phosphoric acid fuel cells, molten carbonate fuel cells, and solid oxide fuel cells (SOFCs). The salient features of an SOFC are all solid construction and high-temperature electrochemical-reaction-based operation, resulting in clean, efficient power generation from a variety of fuels. SOFCs are being developed for a broad range of applications, such as portable electronic devices, automobiles, power generation, and aeronautics.

SiC/SiC composite materials targeted as turbine components for next-generation aero-engines are being investigated at NASA Glenn Research Center. In order to examine damage mechanisms in these materials, SiC/SiC coupons were impacted with 1.59 mm diameter steel spheres at increasing velocities from 115 m/s to 400 m/s. Pulsed thermography, a nondestructive evaluation technique that monitors the thermal response of a sample over time, was utilized to characterize the impact damage. A thermal standard of similar material was fabricated to aid in the interpretation of the thermographic data and to provide information regarding thermography system detection capabilities in 2.4 mm thick SiC/SiC composite materials. Flat bottom holes at various depths with aspect ratios greater than 2.5 were detectable in the thermal images. In addition, the edges of holes at depths of 1.93 mm into the sample were not as resolvable as flat bottom holes closer to the surface. Finally, cooling behavior was characterized in SiC/SiC materials and used to determine impact damage depth within an 8.5% error of a known depth.

Foreign object damage (FOD) behavior of AS800 silicon nitride was determined using four different projectile materials at ambient temperature. The target test specimens rigidly supported were impacted at their centers by spherical projectiles with a diameter of 1.59 mm. Four different types of projectiles were used including hardened steel balls, annealed steel balls, silicon nitride balls, and brass balls. Post-impact strength of each target specimen impacted was determined as a function of impact velocity to better understand the severity of local impact damage. The critical impact velocity where target specimens fail upon impact was highest with brass balls, lowest with ceramic ball, and intermediate with annealed and hardened steel balls. Degree of strength degradation upon impact followed the same order as in the critical impact velocity with respect to projectile materials. For steel balls, hardened projectiles yielded more significant impact damage than annealed counterparts. The most important material parameter affecting FOD was identified as hardness of projectiles and was correlated in terms of critical impact velocity, impact deformation, and impact load.

Thermal barrier coatings will be more aggressively designed to protect gas turbine engine hot-section components in order to meet future engine higher fuel efficiency and lower emission goals. A fundamental understanding of the sintering and thermal cycling induced delamination of thermal barrier coating systems under engine-like heat flux conditions will potentially help to improve the coating temperature capability. In this study, a test approach is established to emphasize the real-time monitoring and assessment of the coating thermal conductivity, which can initially increase under the steady-state high temperature thermal gradient test due to coating sintering, and later decrease under the thermal gradient cyclic test due to coating cracking and delamination. Thermal conductivity prediction models have been established for a ZrO2-(7- 8wt%)Y2O3 model coating system in terms of heat flux, time, and testing temperatures. The coating delamination accumulation is then assessed based on the observed thermal conductivity response under the combined steady-state and cyclic thermal gradient tests. The coating thermal gradient cycling associated delaminations and failure mechanisms under simulated engine heat-flux conditions will be discussed in conjunction with the coating sintering and fracture testing results.

Mechanical behavior of free standing, plasma-sprayed ZrO2-8 wt% Y2O3 thermal barrier coatings, including strength, fracture toughness, fatigue, constitutive relation, elastic modulus, and directionality, has been determined under various loading-specimen configurations. This report presents and describes a summary of mechanical properties of the plasma-sprayed coating material to provide them as a design database.

Ceramic thermal barrier coatings will play an increasingly important role in future gas turbine engines because of their ability to effectively protect the engine components and further raise engine temperatures. Durability of the coating systems remains a critical issue with the ever-increasing temperature requirements. Thermal conductivity increase and coating degradation due to sintering and phase changes are known to be detrimental to coating performance. There is a need to characterize the coating thermal fatigue behavior and temperature limit, in order to potentially take full advantage of the current coating capability. In this study, thermal conductivity and cyclic fatigue behaviors of plasma-sprayed ZrO2-8wt%Y2O3 thermal barrier coatings were evaluated under high temperature, large thermal gradient and thermal cycling conditions. The coating degradation and failure processes were assessed by real-time monitoring of the coating thermal conductivity under the test conditions. The ceramic coating crack initiation and propagation driving forces and failure modes under the cyclic thermal loads will be discussed in light of the high temperature mechanical fatigue and fracture testing results.

The effect of sintering on mechanical and physical properties of free-standing plasma-sprayed ZrO2-8 wt% Y2O3 thermal barrier coatings (TBCs) was determined by annealing them at 1316 C in air. Mechanical and physical properties of the TBCs, including strength, modes I and II fracture toughness, elastic modulus, Poisson s response, density, microhardness, fractography, and phase stability, were determined at ambient temperature as a function of annealing time ranging from 0 to 500 h. All mechanical and physical properties, except for the amount of monoclinic phase, increased significantly in 5 to 100 h and then reached a plateau above 100 h. Annealing resulted in healing of microcracks and pores and in grain growth, accompanying densification of the TBC s body due to the sintering effect. However, an inevitable adverse effect also occurred such that the desired lower thermal conductivity and good expansivity, which makes the TBCs unique in thermal barrier applications, were degraded upon annealing. A model was proposed to assess and quantify all the property variables in response to annealing in a normalized scheme. Directionality of as-sprayed TBCs appeared to have an insignificant effect on their properties, as determined via fracture toughness, microhardness, and elastic modulus measurements.

Tests have shown that modification of chemical compositions can increase the strengths and fracture toughnesses of solid oxide fuel-cell (SOFC) electrolytes. Heretofore, these solid electrolytes have been made of yttria-stabilized zirconia, which is highly conductive for oxygen ions at high temperatures, as needed for operation of fuel cells. Unfortunately yttria-stabilized zirconia has a high coefficient of thermal expansion, low resistance to thermal shock, low fracture toughness, and low mechanical strength. The lack of strength and toughness are especially problematic for fabrication of thin SOFC electrolyte membranes needed for contemplated aeronautical, automotive, and stationary power-generation applications. The modifications of chemical composition that lead to increased strength and fracture toughness consist in addition of alumina to the basic yttria-stabilized zirconia formulations. Techniques for processing of yttria-stabilized zirconia/alumina composites containing as much as 30 mole percent of alumina have been developed. The composite panels fabricated by these techniques have been found to be dense and free of cracks. The only material phases detected in these composites has been cubic zirconia and a alumina: this finding signifies that no undesired chemical reactions between the constituents occurred during processing at elevated temperatures. The flexural strengths and fracture toughnesses of the various zirconia-alumina composites were measured in air at room temperature as well as at a temperature of 1,000 C (a typical SOFC operating temperature). The measurements showed that both flexural strength and fracture toughness increased with increasing alumina content at both temperatures. In addition, the modulus of elasticity and the thermal conductivity were found to increase and the density to decrease with increasing alumina content. The oxygen-ion conductivity at 1,000 C was found to be unchanged by the addition of alumina.

Foreign object damage (FOD) behavior of a gas-turbine grade SiC/SiC ceramic matrix composite (CMC) was determined at 25 and 1316 C, employing impact velocities from 115 to 440 meters per second by 1.59-mm diameter stell-ball projectiles. Two different types of specimen support were used at each temperature: fully supported and partially supported. For a given temperature, the degree of post-impact strength degradation increased with increasing impact velocity, and was greater in a partially supported configuration than in a fully supported one. The elevated-temperature FOD resistance of the composite, particularly under partially supported loading at higher impact velocities greater than or equal to 350 meters per second, was significantly less than the ambient-temperature counterpart, attributed to a weakening effect of the composite. For fully supported loading, frontal contact stress played a major role in generating composite damage; whereas, for partially supported loading, both frontal contact and backside bending stresses were combined sources of damage generation. The SiC/SiC composite was able to survive higher energy impacts without complete structural failure but suffered more strength affecting damage from low energy impacts than AS800 and SN282 silicon nitrides.

Ceramic thermal barrier coatings will play an increasingly important role in future gas turbine engines because of their ability to effectively protect the engine components and further raise engine temperatures. Durability of the coating systems remains a critical issue with the ever-increasing temperature requirements. Thermal conductivity increase and coating degradation due to sintering and phase changes are known to be detrimental to coating performance. There is a need to characterize the coating behavior and temperature limits, in order to potentially take full advantage of the current coating capability, and also accurately assess the benefit gained from advanced coating development. In this study, thermal conductivity behavior and cyclic durability of plasma-sprayed ZrO2-8wt%Y2O3 thermal barrier coatings were evaluated under laser heat-flux simulated high temperature, large thermal gradient and thermal cycling conditions. The coating degradation and failure processes were assessed by real-time monitoring of the coating thermal conductivity under the test conditions. The ceramic coating crack propagation driving forces and resulting failure modes will be discussed in light of high temperature mechanical fatigue and fracture testing results.

Foreign object damage (FOD) behavior of two commercial gas-turbine grade silicon nitrides, AS800 and SN282, was determined at ambient temperature through strength testing of flexure test specimens impacted by steel ball projectiles with a diameter of 1.59 mm in a velocity range from 220 to 440 m/s. AS800 silicon nitride exhibited a greater FOD resistance than SN282, primarily due to its greater value of fracture toughness (K(sub lc)). The use of an additional equiaxed, fine-grained silicon nitride (NC132) showed that fracture toughness was a key material parameter affecting FOD resistance. The observed damages generated by projectile impact were typically in the forms of well- or ill-developed ring and cone cracks with little presence of radial cracks.

Thermal barrier coatings will be more aggressively designed to protect gas turbine engine hot-section components in order to meet future engine higher fuel efficiency and lower emission goals. There is a need to characterize the fundamental sintering and fracture behavior of the current ZrO2-(7 to 8)wt%Y2O3 coating, in order to fully take advantage of the coating capability. In addition, a thorough evaluation of the coating behavior and temperature limits will be useful for more accurately assessing the benefit gained from future advanced coating systems. In this study, the sintering behavior of plasma-sprayed ZrO2-8wt%Y2O3 coatings was systematically investigated as a function of temperature and time using a dilatometer in the temperature range of 1200-1500 C. The coating sintering kinetics obtained by dilatometry were compared with the coating thermal conductivity increase kinetics, determined by a steady-state laser heat-flux testing approach, under high temperature and thermal gradient sintering conditions. The mode I, mode II, and mixed mode I-mode II fracture behavior of as-processed and sintering-annealed coatings was determined in asymmetric flexure loading at ambient and elevated temperatures in order to evaluate the coating sintering effects on the fracture envelope of K(sub I) versus K(sub II). The coating thermal conductivity cyclic response associated with the interface delamination of the coating systems under simulated engine heat-flux conditions will be discussed in conjunction with the sintering and fracture testing results.

Ceramic thermal/environmental barrier coatings for SiC-based ceramics will play an increasingly important role in future gas turbine engines because of their ability to effectively protect the engine components and further raise engine temperatures. However, the coating durability remains a major concern with the ever-increasing temperature requirements. Currently, advanced T/EBC systems, which typically include a high temperature capable zirconia- (or hahia-) based oxide top coat (thermal barrier) on a less temperature capable mullite/barium-strontium-aluminosilicate (BSAS)/Si inner coat (environmental barrier), are being developed and tested for higher temperature capability Sic combustor applications. In this paper, durability of several thermal/environmental barrier coating systems on SiC/SiC ceramic matrix composites was investigated under laser simulated engine thermal gradient cyclic, and 1650 C (3000 F) test conditions. The coating cracking and delamination processes were monitored and evaluated. The effects of temperature gradients and coating configurations on the ceramic coating crack initiation and propagation were analyzed using finite element analysis (FEA) models based on the observed failure mechanisms, in conjunction with mechanical testing results. The environmental effects on the coating durability will be discussed. The coating design approach will also be presented.

An accelerated-testing methodology has been developed for measuring the slow-crack-growth (SCG) behavior of brittle materials. Like the prior methodology, the accelerated-testing methodology involves dynamic fatigue ( constant stress-rate) testing, in which a load or a displacement is applied to a specimen at a constant rate. SCG parameters or life prediction parameters needed for designing components made of the same material as that of the specimen are calculated from the relationship between (1) the strength of the material as measured in the test and (2) the applied stress rate used in the test. Despite its simplicity and convenience, dynamic fatigue testing as practiced heretofore has one major drawback: it is extremely time-consuming, especially at low stress rates. The present accelerated methodology reduces the time needed to test a specimen at a given rate of applied load, stress, or displacement. Instead of starting the test from zero applied load or displacement as in the prior methodology, one preloads the specimen and increases the applied load at the specified rate (see Figure 1). One might expect the preload to alter the results of the test and indeed it does, but fortunately, it is possible to account for the effect of the preload in interpreting the results. The accounting is done by calculating the normalized strength (defined as the strength in the presence of preload the strength in the absence of preload) as a function of (1) the preloading factor (defined as the preload stress the strength in the absence of preload) and (2) a SCG parameter, denoted n, that is used in a power-law crack-speed formulation. Figure 2 presents numerical results from this theoretical calculation.

Alumina-reinforced zirconia composites, used as electrolyte materials for solid oxide fuel cells, were fabricated by hot pressing 10 mol percent yttria-stabilized zirconia (10-YSZ) reinforced with two different forms of alumina particulates and platelets each containing 0 to 30 mol percent alumina. Major mechanical and physical properties of both particulate and platelet composites including flexure strength, fracture toughness, slow crack growth, elastic modulus, density, Vickers microhardness, thermal conductivity, and microstructures were determined as a function of alumina content either at 25 C or at both 25 and 1000 C. Flexure strength and fracture toughness at 1000 C were maximized with 30 particulate and 30 mol percent platelet composites, respectively, while resistance to slow crack growth at 1000 C in air was greater for 30 mol percent platelet composite than for 30 mol percent particulate composites.

Mechanical testing for Pyroceram (trademark) 9606 glass-ceramic fabricated by Corning was conducted to determine mechanical properties of the material including slow crack growth.Valid testing was not achieved in tension, compression, and shear testing due to inappropriate test specimen configurations provided and primarily due to the existence of fortified layer( in tension).

Strength, fracture toughness and fatigue behavior of free-standing thick thermal barrier coatings of plasma-sprayed ZrO2-8wt % Y2O3 were determined at ambient and elevated temperatures in an attempt to establish a database for design. Strength, in conjunction with deformation (stress-strain behavior), was evaluated in tension (uniaxial and trans-thickness), compression, and uniaxial and biaxial flexure; fracture toughness was determined in various load conditions including mode I, mode II, and mixed modes I and II; fatigue or slow crack growth behavior was estimated in cyclic tension and dynamic flexure loading. Effect of sintering was quantified through approaches using strength, fracture toughness, and modulus (constitutive relations) measurements. Standardization issues on test methodology also was presented with a special regard to material's unique constitutive relations.

Foreign object damage (FOD) behavior of two commercial gas-turbine-grade silicon nitrides, AS800 and SN282, was determined at ambient temperature through postimpact strength testing of disks impacted by steel ball projectiles with a diameter of 1.59 mm in a velocity range from 115 to 440 m/s. AS800 silicon nitride exhibited a greater FOD resistance than SN282, primarily due to its greater value of fracture toughness (k(sub Ic)). The critical impact velocity V(sub c) for which the corresponding postimpact strength was the lowest was V(sub c) approximately equal to 440 and 300 m/s AS800 and SN282, respectively. A unique lower strength regime was typified for both silicon nitrides depending on impact velocity and was attributed to significant radial cracking. The damage generated by projectile impact was typically in the form of ring, radial, and cone cracks with their severity and combination being dependent on impact velocity. Unlike the thick (4 millimeters) flexure bar specimens used in our previous studies, the thin (2 millimeter) disk target specimen exhibited a unique back-side radial cracking on the reverse side just beneath the impact sites at and above impact velocities of 160 meters per second for SN282 and 220 meters per second AS800.

Dense and crack-free 10-mol%-yttria-stabilized zirconia (10YSZ)-alumina composites, containing 0 to 30 mol% of alumina, have been fabricated by hot pressing. Release of pressure before onset of cooling was crucial in obtaining crack-free material. Hot pressing at 1600 C resulted in the formation of ZrC by reaction of zirconia with grafoil. However, no such reaction was observed at 1500 C. Cubic zirconia and -alumina were the only phases detected from x-ray diffraction indicating no chemical reaction between the composite constituents during hot pressing. Microstructure of the composites was analyzed by scanning electron microscopy and transmission electron microscopy. Density and elastic modulus of the composites followed the rule-of-mixtures. Addition of alumina to 10YSZ resulted in lighter, stronger, and stiffer composites by decreasing density and increasing strength and elastic modulus.

Both interlaminar and in-plane shear strengths of a unidirectional Hi-Nicalon(TM) fiber-reinforced barium strontium aluminosilicate (SiC/BSAS) composite were determined at 1100 C in air as a function of test rate using double notch shear test specimens. The composite exhibited a significant effect of test rate on shear strength, regardless of orientation which was either in interlaminar or in in-plane direction, resulting in an appreciable shear-strength degradation of about 50 percent as test rate decreased from 3.3 10(exp -1) mm/s to 3.3 10(exp -5) mm/s. The rate dependency of composite's shear strength was very similar to that of ultimate tensile strength at 1100 C observed in a similar composite (2-D SiC/BSAS) in which tensile strength decreased by about 60 percent when test rate varied from the highest (5 MPa/s) to the lowest (0.005 MPa/s). A phenomenological, power-law slow crack growth formulation was proposed and formulated to account for the rate dependency of shear strength of the composite.

In this paper, surface cracking and interface reactions of a BSAS coating and a multi-layer ZrO2-8wt%Y2O3 and mullite/BSAS/Si thermal and environmental barrier coating system on SiC/SiC ceramic matrix composites were characterized after long-term combined laser thermal gradient and furnace cyclic tests in a water vapor containing environment. The surface cracking was analyzed based on the coating thermal gradient sintering behavior and thermal expansion mismatch stress characteristics under the thermal cyclic conditions. The interface reactions, which were largely enhanced by the coating surface cracking in the water vapor environment, were investigated in detail, and the reaction phases were identified for the coating system after the long-term exposure. The accelerated coating delamination failure was attributed to the increased delamination driving force under the thermal gradient cyclic loading and the reduced interface adhesion due to the detrimental interface reactions.

The mixed-mode fracture behavior of plasma-sprayed ZrO2-8 wt% Y2O3 thermal barrier coatings was determined in air at 25 and 1316 C in asymmetric four-point flexure with single edge v-notched beam (SEVNB) test specimens. The mode I fracture toughness was found to be K(sub Ic) = 1.15 plus or minus 0.07 and 0.98 plus or minus 0.13 MPa the square root of m, respectively, at 25 and 1316 C. The respective mode II fracture toughness values were K(sub IIc) = 0.73 plus or minus 0.10 and 0.65 plus or minus 0.04 MPa the square root of m. Hence, there was an insignificant difference in either K(sub Ic or K(sub IIc) between 25 and 1316 C for the coating material, whereas there was a noticeable distinction between K(sub Ic) and K(sub IIc), resulting in K(sub IIc) per K(sub Ic) = 0.65 at both temperatures. The empirical mixed-mode fracture criterion best described the coatings' mixed-mode fracture behavior among the four mixed-mode fracture theories considered. The angle of crack propagation was in reasonable agreement with the minimum strain energy density criterion. The effect of the directionality of the coating material in on K(sub Ic) was observed to be insignificant, while its sintering effect at 1316 C on K(sub Ic) was significant.

Various electrolyte materials for solid oxide fuel cells were fabricated by hot pressing 10 mol% yttria-stabilized zirconia (10-YSZ) reinforced with two different forms of alumina particulates and platelets each containing 0 to 30 mol% alumina. Flexure strength and fracture toughness of platelet composites were determined as a function of alumina content at 1000 C in air and compared with those of particulate composites determined previously. In general, elevated-temperature strength and fracture toughness of both composite systems increased with increasing alumina content. For a given alumina content, flexure strength of particulate composites was greater than that of platelet composites at higher alumina contents (greater than or equal to 20 mol%), whereas, fracture toughness was greater in platelet composites than in particulate composites, regardless of alumina content. The results of slow crack growth (SCG) testing, determined at 1000 C via dynamic fatigue testing for three different composites including 0 mol% (10-YSZ matrix), 30 mol % particulate and 30 mol% platelet composites, showed that susceptibility to SCG was greatest with SCG parameter n = 6 to 8 for both 0 and 30 mol% particulate composites and was least with n = 33 for the 30 mol% platelet composite.

Advanced ceramic thermal harrier coatings will play an increasingly important role In future gas turbine engines because of their ability to effectively protect the engine components and further raise engine temperatures. However, the coating durability issue remains a major concern with the ever-increasing temperature requirements. In this paper, thermal cyclic response and delamination failure modes of a ZrO2-8wt%Y2O3 and mullite/BSAS thermaVenvironmenta1 barrier coating system on SiC/SiC ceramic matrix composites were investigated using a laser high-heat-flux technique. The coating degradation and delamination processes were monitored in real time by measuring coating apparent conductivity changes during the cyclic tests under realistic engine temperature and stress gradients, utilizing the fact that delamination cracking causes an apparent decrease in the measured thermal conductivity. The ceramic coating crack initiation and propagation driving forces under the cyclic thermal loads, in conjunction with the mechanical testing results, will be discussed.

The mode I, mode II, and combined mode I-mode II fracture behavior of ZrO2- 8wt%Y2O3 thermal barrier coatings was determined in asymmetric flexure loading at both ambient and elevated temperatures. Precracks were introduced in test specimens using the single-edge-v-notched beam (SEVNB) method incorporated with final diamond polishing to achieve sharp crack tips. A fracture envelope of KI versus KII was determined for the coating material at ambient and elevated temperatures. Propagation angles of fracture as a function of K(sub I)/K(sub II) were also determined. The mixed-mode fracture behaviors of the coating material were compared with those of monolithic advanced ceramics determined previously. The mixed-mode fracture behavior of the plasma-sprayed thermal barrier coating material was predicted in terms of fracture envelope and propagation angle using mixed-mode fracture theories.

Foreign object damage (FOD) behavior of two commercial gas-turbine grade silicon nitrides, AS800 and SN282, was determined at ambient temperature through post-impact strength testing for thin disks impacted by steel-ball projectiles with a diameter of 1.59 mm in a velocity range from 115 to 440 m/s. AS800 silicon nitride exhibited a greater FOD resistance than SN282, primarily due to its greater value of fracture toughness (K(sub IC)). The critical impact velocity in which the corresponding post-impact strength yielded the lowest value was V(sub c) approx. 440 and 300 m/s for AS800 and SN282, respectively. A unique lower-strength regime was typified for both silicon nitrides depending on impact velocity, attributed to significant radial cracking. The damages generated by projectile impact were typically in the forms of ring, radial, and cone cracks with their severity and combination being dependent on impact velocity. Unlike thick (3 mm) flexure bar specimens used in the previous studies, thin (2 mm) disk target specimens exhibited a unique backside radial cracking occurring on the reverse side just beneath the impact sites at and above impact velocity of 160 and 220 m/s for SN282 and AS800, respectively.

In this paper, surface cracking and interface reactions of a BSAS coating and a multi-layer ZTO2-8wt%Y2O3 and mullite/BSAS/Si thermal and environmental barrier coating system on SiC/SiC ceramic matrix composites were characterized after long-term combined laser thermal gradient and furnace cyclic tests in a water vapor containing environment. The surface cracking was analyzed based on the coating thermal gradient sintering behavior and thermal expansion mismatch stress characteristics under the thermal cyclic conditions. The interface reactions, which were largely enhanced by the coating surface cracking in the water vapor environment, were investigated in detail, and the reaction phases were identified for the coating system after the long- term exposure. The accelerated coating delamination failure was attributed to the increased delamination driving force under the thermal gradient cyclic loading and the reduced interface adhesion due to the detrimental interface reactions.

Foreign object damage (FOD) behavior of two commercial gas-turbine grade silicon nitrides, AS800 and SN282, was determined at ambient temperature through strength testing of flexure test specimens impacted by steel-ball projectiles with a diameter of 1.59 mm in a velocity range from 220 to 440 m/s. AS800 silicon nitride exhibited a greater FOD resistance than SN282, primarily due to its greater value of fracture toughness (K(sub IC)). Additionally, the FOD response of an equiaxed, fine-grained silicon nitride (NC132) was also investigated to provide further insight. The NC132 silicon nitride exhibited the lowest fracture toughness of the three materials tested, providing further evidence that K(sub IC) is a key material parameter affecting FOD resistance. The observed damage generated by projectile impact was typically in the forms of well- or ill-developed ring or cone cracks with little presence of radial cracks.

The previously determined life prediction analysis based on an exponential crack-velocity formulation was examined using a variety of experimental data on advanced structural ceramics tested under constant stress and cyclic stress loading at ambient and elevated temperatures. The data fit to the relation between the time to failure and applied stress (or maximum applied stress in cyclic loading) was very reasonable for most of the materials studied. It was also found that life prediction for cyclic stress loading from data of constant stress loading in the exponential formulation was in good agreement with the experimental data, resulting in a similar degree of accuracy as compared with the power-law formulation. The major limitation in the exponential crack-velocity formulation, however, was that the inert strength of a material must be known a priori to evaluate the important slow-crack-growth (SCG) parameter n, a significant drawback as compared with the conventional power-law crack-velocity formulation.

Various electrolyte materials for solid oxide fuel cells were fabricated by hot pressing 10 mol% yttria-stabilized zirconia (10-YSZ) reinforced with two different forms of alumina, particulates and platelets, each containing 0 to 30 mol% alumina. Flexure strength and fracture toughness of both particulate and platelet composites at ambient temperature increased with increasing alumina content, reaching a maximum at 30 mot% alumina. For a given alumina content, strength of particulate composites was greater than that of platelet composites, whereas, the difference in fracture toughness between the two composite systems was negligible. No virtual difference in elastic modulus and density was observed for a given alumina content between particulate and platelet composites. Thermal cycling up to 10 cycles between 200 to 1000 C did not show any effect on strength degradation of the 30 mol% platelet composites, indicative of negligible influence of CTE mismatches between YSZ matrix and alumina grains.

Ultimate tensile strength of five different continuous fiber-reinforced ceramic composites, including SiC/BSAS (2D 2 types), SiC/MAS-5 (2D), SiC/SiC (2D enhanced), and C/SiC(2D) was determined as a function of test rate at I 100 to 1200 'C in air. All five composite materials exhibited a significant dependency of ultimate strength on test rate such that the ultimate strength decreased with decreasing test rate, similar to the behavior observed in many advanced monolithic ceramics at elevated temperatures. The application of the preloading technique as well as the prediction of life from one loading configuration (constant stress rate) to another (constant stress loading) for SiC/BSAS suggested that the overall macroscopic failure mechanism of the composites would be the one governed by a power-law type of damage evolution/accumulation, analogous to slow crack growth commonly observed in advanced monolithic ceramics.

High-temperature creep behavior of ceramics is characterized by nonlinear time-dependent responses, asymmetric behavior in tension and compression, and nucleation and coalescence of voids leading to creep rupture. Moreover, creep rupture experiments show considerable scatter or randomness in fatigue lives of nominally equal specimens. To capture the nonlinear, asymmetric time-dependent behavior, the standard linear viscoelastic solid model is modified. Nonlinearity and asymmetry are introduced in the volumetric components by using a nonlinear function similar to a hyperbolic sine function but modified to model asymmetry. The nonlinear viscoelastic model is implemented in an ABAQUS user material subroutine. To model the random formation and coalescence of voids, each element is assigned a failure strain sampled from a lognormal distribution. An element is deleted when its volumetric strain exceeds its failure strain. Element deletion has been implemented within ABAQUS. Temporal increases in strains produce a sequential loss of elements (a model for void nucleation and growth), which in turn leads to failure. Nonlinear viscoelastic model parameters are determined from uniaxial tensile and compressive creep experiments on silicon nitride. The model is then used to predict the deformation of four-point bending and ball-on-ring specimens. Simulation is used to predict statistical moments of creep rupture lives. Numerical simulation results compare well with results of experiments of four-point bending specimens. The analytical model is intended to be used to predict the creep rupture lives of ceramic parts in arbitrary stress conditions.

Solid oxide fuel cells (SOFC) are being developed for various applications in the automobile, power-generation, and aeronautics industries. Recently, the NASA Glenn Research Center has been exploring the possibility of using SOFC's for aeropropulsion under its Zero Carbon Dioxide Emission Technology (ZCET) Program. 10-mol% yttriastabilized zirconia (10YSZ) is a very good anionic conductor at high temperatures and is, therefore, used as an oxygen solid electrolyte in SOFC. However, it has a high thermal expansion coefficient, low thermal shock resistance, low fracture toughness, and poor mechanical strength. For aeronautic applications, the thin ceramic electrolyte membrane of the SOFC needs to be strong and tough. Therefore, we have been investigating the possibility of enhancing the strength and fracture toughness of the 10YSZ electrolyte without degrading its electrical conductivity to an appreciable extent. We recently demonstrated that the addition of alumina to zirconia electrolyte increases its strength as well as its fracture toughness. Zirconia-alumina composites containing 0 to 30 mol% of alumina were fabricated by hot pressing. The hot pressing procedure was developed and various hot pressing parameters were optimized, resulting in dense, crackfree panels of composite materials. Cubic zirconia and a-alumina were the only phases detected, indicating that there was no chemical reaction between the constituents during hot pressing at elevated temperatures. Flexure strength sf and fracture toughness K(sub IC) of the various zirconia-alumina composites were measured at room temperature as well as at 1000 C in air. Both properties showed systematic improvement with increased alumina addition at room temperature and at 1000 C. Use of these modified electrolytes with improved strength and fracture toughness should prolong the life and enhance the performance of SOFC in aeronautics and other applications.

Brittle materials, ceramics, are candidate materials for a variety of structural applications for a wide range of temperatures. However, the process of slow crack growth, occurring in any loading configuration, limits the service life of structural components. Therefore, it is important to accurately determine the slow crack growth parameters required for component life prediction using an appropriate test methodology. This test methodology also should be useful in determining the influence of component processing and composition variables on the slow crack growth behavior of newly developed or existing materials, thereby allowing the component processing and composition to be tailored and optimized to specific needs. Through the American Society for Testing and Materials (ASTM), the authors recently developed two test methods to determine the life prediction parameters of ceramics. The two test standards, ASTM 1368 for room temperature and ASTM C 1465 for elevated temperatures, were published in the 2001 Annual Book of ASTM Standards, Vol. 15.01. Briefly, the test method employs constant stress-rate (or dynamic fatigue) testing to determine flexural strengths as a function of the applied stress rate. The merit of this test method lies in its simplicity: strengths are measured in a routine manner in flexure at four or more applied stress rates with an appropriate number of test specimens at each applied stress rate. The slow crack growth parameters necessary for life prediction are then determined from a simple relationship between the strength and the applied stress rate. Extensive life prediction testing was conducted at the NASA Glenn Research Center using the developed ASTM C 1368 test method to determine the life prediction parameters of a glass-ceramic material that the Navy will use for radome applications.

The life prediction analysis based on an exponential crack velocity formulation was examined using a variety of experimental data on glass and advanced structural ceramics in constant stress-rate ("dynamic fatigue") and preload testing at ambient and elevated temperatures. The data fit to the strength versus In (stress rate) relation was found to be very reasonable for most of the materials. It was also found that preloading technique was equally applicable for the case of slow crack growth (SCG) parameter n > 30. The major limitation in the exponential crack velocity formulation, however, was that an inert strength of a material must be known priori to evaluate the important SCG parameter n, a significant drawback as compared to the conventional power-law crack velocity formulation.

The strengths of three continuous fiber-reinforced ceramic composites, including SiC/CAS-II, SiC/MAS-5 and SiC/SiC, were determined as a function of test rate in air at 1100 to 1200 C. All three composite materials exhibited a strong dependency of strength on test rate, similar to the behavior observed in many advanced monolithic ceramics at elevated temperatures. The application of the preloading technique as well as the prediction of life from one loading configuration (constant stress-rate) to another (constant stress loading) suggested that the overall macroscopic failure mechanism of the composites would be the one governed by a power-law type of damage evolution/accumulation, analogous to slow crack growth commonly observed in advanced monolithic ceramics. It was further found that constant stress-rate testing could be used as an alternative to life prediction test methodology even for composite materials, at least for short range of lifetimes and when ultimate strength is used as the failure criterion.

Thermal fatigue and fracture behavior of plasma-sprayed ceramic thermal barrier coatings has been investigated under high heat flux and thermal cyclic conditions. The coating crack propagation is studied under laser heat flux cyclic thermal loading, and is correlated with dynamic fatigue and strength test results. The coating stress response and inelasticity, fatigue and creep interactions, and interface damage mechanisms during dynamic thermal fatigue processes are emphasized.