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NASA NTRS2002

Thermal Gradient Cyclic Behavior of a Thermal/Environmental Barrier Coating System on SiC/SiC Ceramic Matrix Composites

Thermal barrier and environmental barrier coatings (TBCs and EBCs) will play a crucial role in future advanced gas turbine engines because of their ability to significantly extend the temperature capability of the ceramic matrix composite (CMC) engine components in harsh combustion environments. In order to develop high performance, robust coating systems for effective thermal and environmental protection of the engine components, appropriate test approaches for evaluating the critical coating properties must be established. In this paper, a laser high-heat-flux, thermal gradient approach for testing the coatings will be described. Thermal cyclic behavior of plasma-sprayed coating systems, consisting of ZrO2-8wt%Y2O3 thermal barrier and NASA Enabling Propulsion Materials (EPM) Program developed mullite+BSAS/Si type environmental barrier coatings on SiC/SiC ceramic matrix composites, was investigated under thermal gradients using the laser heat-flux rig in conjunction with the furnace thermal cyclic tests in water-vapor environments. The coating sintering and interface damage were assessed by monitoring the real-time thermal conductivity changes during the laser heat-flux tests and by examining the microstructural changes after the tests. The coating failure mechanisms are discussed based on the cyclic test results and are correlated to the sintering, creep, and thermal stress behavior under simulated engine temperature and heat flux conditions.

Zhu, Dongming↗
NASA NTRS2002

High Temperature Si-doped BN Interphases for Woven SiC/SiC Composites

The hydrolytic stability of high-temperature deposited Si-doped BN has been shown in the past to be superior in comparison to "pure" BN processed at similar or even higher temperatures. This type of material would be very desirable as a SiC/SiC composite interphase that is formed by chemical infiltration into multi-ply woven preform. However, due to rapid deposition on the preform outer surface at the high processing temperature, this has proven very difficult. To overcome this issue, single plies of woven fabric were infiltrated with Si-doped BN. Three composite panels of different SiC fiber types were fabricated with Si-doped BN interphases including Sylramic, Hi-Nicalon Type S and Sylramic-iBN fiber-types. The latter fiber-type possesses a thin in-situ grown BN layer on the fiber surface. High Si contents (approx. 7 to 10 a/o) and low oxygen contents (less than 1 a/o) were achieved. All three composite systems demonstrated reasonable debonding and sliding properties. The coated Sylramic fabric and composites were weak due to fiber degradation apparently caused during interphase processing by the formation of TiN crystals on the fiber surface. The Hi-Nicalon Type S composites with Si-doped BN interphase were only slightly weaker than Hi-Nicalon Type S composites with conventional BN when the strength on the load-bearing fibers at failure was compared. On the other hand, the Sylramic-iBN fabric and composites with Si-doped BN showed excellent composite and intermediate temperature stress-rupture properties. Most impressive was the lack of any significant interphase oxidation on the fracture surface of stress-ruptured specimens tested well above matrix cracking at 815C.

Morscher, Gregory N.↗
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 NTRS2002

High Temperature Tensile Properties and Fatigue Behavior of a Melt-Infiltrated SiC/SiC Composite

High temperature fatigue behavior of a woven, SiC/SiC ceramic matrix composite (CMC) was investigated in air at two temperatures. The reinforcement for the CMC consisted of 5HS Sylramic(Trademark) fabric with a [0deg/90deg]4s lay-up. The SiC matrix material was infiltrated into the fiber-preform with a slurry-cast, melt-infiltration process. Tensile and fatigue test specimens were machined from the CMC plates. Initially tensile tests were conducted to obtain the average values of tensile properties at 1038 and 1204 C. Subsequently, low-cycle fatigue (LCF) tests with zero and two-hour hold-times at the maximum stress were conducted at the same two temperatures. Fatigue life data generated in the LCF tests were used to determine the geometric mean fatigue lives. In this paper, the tensile behavior and the fatigue durability of the CMC determined under different loading conditions are documented. In addition, reductions observed in the cyclic lives of the composite due to the two hour hold-time at maximum tensile stress are discussed.

Kalluri, Sreeramesh↗
NASA NTRS2002

Hoop Tensile Characterization Of SiC/SiC Cylinders Fabricated From 2D Fabric

Tensile stress-strain properties in the hoop direction were obtained for 100-mm diameter SiC/SiC cylinders using ring specimens machined from the cylinder ends. The cylinders were fabricated from 2D balanced fabric with several material variants, including wall thickness (6, 8, and 12 plies), Sic fiber type (Sylramic, Sylramic-iBN, Hi-Nicalon, and Hi-Nicalon S), fiber sizing type, and matrix type (full CVI Sic, and partial CVI plus melt-infiltrated SiC-Si). Fiber ply splices existed in the all the hoops. Tensile hoop measurements were made at room temperature and 1200 C using hydrostatic ring test facilities. The hoop results are compared with in-plane data measured on flat panels using same material variants, but containing no splices.

Verrilli, Michael J.↗
NASA NTRS2003

Comparison of Matrix Cracking in Melt-Infiltrated SiC/SiC Composites with 3D and 2D-Woven Orthogonal Architectures

Acoustic emission techniques combined with microstructural observations were used to determine the dependence of through thickness matrix cracking (TTMC) on in-plane tensile stress for melt infiltrated Sylramic fiber-based SIC/SiC composite panels with various 3D-woven orthogonal fiber architectures. Results were compared with prior TTMC results from similar panels with 2D woven orthogonal architectures.Both data sets were analysed on the basis that the source for TTMC originated in the 90 degree or Z-fiber tows.

Morscher, Gregory N.↗
NASA NTRS2003

Matrix Cracking in 3D Orthogonal Melt-Infiltrated SiC/SiC Composites with Various Z-Fiber Types

The occurrence of matrix cracks in melt-infiltrated SiC/SiC composites with a 3D orthogonal architecture was determined at room temperature for specimens tested in tension oriented in the X-direction (parallel to Z-bundle weave direction) and Y-direction (perpendicular to Z-bundle weave direction) and Y-direction (perpendicular to Z-bundle weave direction). The fiber-types were Sylramic and Sylramic-IBN in the X and Y-directions and lower modulus ZMI, T300, and rayon in the Z-direction. Acoustic emission (AE) was used to monitor the matrix cracking activity. For Y-direction composites, the AE data was used to determine the exact (+/- 0.25 mm) location where matrix cracks occurred in the 3D orthogonal architecture. This enabled the determination of the stress-dependent matrix crack distributions for small but repeatable matrix rich 'unidirectional' and the matrix poor 'cross-ply' regions within the architecture. It was found that matrix cracking initiated at very low stresses (approx. 40 MPa) in the 'unidirectional' regions for the largest z-direction fiber tow composites. Decreasing the size of the z-fiber bundle, increased the stress for matrix cracking in the 'unidirectional' regions. Matrix cracking in the 'cross-ply' regions always occurred at higher stresses than in 'unidirectional' regions, and the stress-dependent matrix crack distribution of the 'cross-ply' regions was always over a wider stress-range than the 'unidirectional' regions. For composites tested in the X-direction, a lower elastic modulus and a narrower and lower stress-range for matrix cracking were observed compared to composites tested in the Y-direction.

Morscher, Gregory N.↗
NASA NTRS2003

SiC/SiC Life Modeling at Intermediate Temperatures under NASA UEET

Within the NASA UEET program, physics-based residual strength and rupture life models are being developed for a variety of time-temperature-stress-environment conditions for SiC/SiC components such as combustor liners and vanes. During service, a tensile stress condition that could be life-limiting typically occurs on the 'cold side' of these components due to thermal gradients and attachment schemes. An intermediate temperature (600 to 1000 C) stress-rupture model has been developed based on the underlying physical processes, i.e., oxygen penetration through matrix cracks, oxidation of the BN interphase, and subsequent fiber-fiber fusion within crack-bridging tows that eventually fail in time due to time-dependent strength degradation of the weakest fibers. Modifications to the model will be discussed to incorporate different environmental conditions as well as changes in oxidation kinetics due to improved interphase concepts.

Morscher, Gregory N.↗
NASA NTRS2004

SiC/SiC Composites for Applications Above 2600 F

Using data from panels with 2D woven architectures,t his presentation describes progress in identifying advanced constituent materials and processes for achieving a high conductivity SiC/SiC composite system with long-term structural life under oxidizing conditions at 2600 degrees F. A key factor for this progress is the development of approaches at NASA GRC that allow the constituent SiC fiber and SiC matrix to display high thermal conductivity, high creep-rupture resistance and high microstructural stability at temperatures above 3000 degree F. Another important factor is the avoidance of free silicon in the SiC matrix, thereby providing the composites with the capability for extended service above the silicon melting point (2550 degrees F). The effects of utilizing various materials and processes for the SiC matrix are presented and discussed.

DiCarlo, James A.↗
NASA NTRS2004

An Assessment of Variability in the Average Tensile Properties of a Melt-Infiltrated SiC/SiC Composite

Woven SiC/SiC Ceramic Matrix Composites (CMCs), manufactured by the slurry-cast, melt-infiltration process are under consideration as combustor liner materials in aircraft gas turbine engines. Tensile properties (elastic modulus, proportional limit strength, in-plane tensile strength and strain to failure) of the CMC, manufactured during two separate time periods (9/99 and 1/01) were determined at 816 and 1024 C by conducting tensile tests on specimens machined from the CMC plates. A total of 24 tensile tests were conducted for each temperature and CMC variant combination. In this study average tensile properties of the two cMC variants were statistically compared to evaluate significant differences, if any, within the CMC's properties.

Kalluri, Sreeramesh↗
NASA NTRS2004

Computation of Variability in the Average Thermal and Mechanical Properties of a Melt-infiltrated Sic/sic Composite

Thermal conductivity and tensile properties (elastic modulus, proportional limit strength, inplane tensile strength, and strain to failure) of a SiC/SiC composite were experimentally determined at 816 and 1204 C. Tests were performed at room temperature on the same material to obtain interlaminar shear and tensile strength. For each thermal and mechanical property 24 tests were conducted to capture the variation. A random sampling method was used to quantify the variability exhibited by the mean values of the thermal and mechanical properties. The minimum number of tests required to characterize the mean value of each thermal or mechanical property for the composite was determined by varying the group size of the random sample.

Kalluri, Sreeramesh↗
NASA NTRS2004

Issues on Fabrication and Evaluation of SiC/SiC Tubes With Various Fiber Architectures

SiC/SiC engine components, high-modulus Sylramic-iBN SiC fiber tows were used to form nine different tubular architectural preforms with 13 mm (0.5 in.) inner diameter and lengths of approx. 75 and 230 mm (approx. 3 and approx, 9 in.). The thin-walled preforms were then coated with a BN interphase and densified with a hybrid SiC matrix using nearly the same process steps previously established for slurry-cast melt-infiltrated Sylramic-iBN/BN/SiC flat panels. The as-fabricated CMC tubes were microstructurally evaluated and tested for tensile hoop and flexural behavior, and some of the tubes were also tested in a low-pressure burner rig test with a high thru-thickness thermal gradient. To date, four general tube scale-up issues have been identified: greater CVI deposits on outer wall than inner wall; increased ply thickness and reduced fiber fraction; poor test standards for accurately determining the hoop strength of a small-diameter tube; and poor hoop strength for architectures with seams or ply ends. The underlying mechanisms and possible methods for their minimization are discussed.

Yun, H. M.↗
NASA NTRS2005

Foreign Object Damage Resistance of Uncoated SiC/SiC Composites

2-D 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 steel-ball projectiles at projectile velocities ranging from 110 m/s to 400 m/s. The extent of substrate damage with increasing projectile velocity was imaged and analyzed using optical microscopy and nondestructive evaluation (NDE) methods. The impacted specimens were flexure and tensile tested at room temperature to determine their residual mechanical properties. Results indicate that as the projectile velocity increases, internal damage in the target material also increases and the mechanical properties degrade. At velocities > 300 m/s, the projectile penetrates through the target material, but it still retains approx. 50% ultimate strength of the as-fabricated composites and exhibits non-brittle failure.

Bhatt, R. T.↗
NASA NTRS2005

The Effect of Fiber Architecture on Matrix Cracking in Sic/sic Cmc's

Applications incorporating silicon carbide fiber reinforced silicon carbide matrix composites (CMC's) will require a wide range of fiber architectures in order to fabricate complex shape. The stress-strain response of a given SiC/SiC system for different architectures and orientations will be required in order to design and effectively life-model future components. The mechanism for non-linear stress-strain behavior in CMC's is the formation and propagation of bridged-matrix cracks throughout the composite. A considerable amount of understanding has been achieved for the stress-dependent matrix cracking behavior of SiC fiber reinforced SiC matrix systems containing melt-infiltrated Si. This presentation will outline the effect of 2D and 3D architectures and orientation on stress-dependent matrix-cracking and how this information can be used to model material behavior and serve as the starting point foe mechanistic-based life-models.

Morscher, Gregory N.↗
NASA NTRS2005

Comparison of Elevated Temperature Tensile Properties and Fatigue Behavior of Two Variants of a Woven SiC/SiC Composite

Tensile properties (elastic modulus, proportional limit strength, in-plane tensile strength, and strain at failure) of two variants of a woven SiC/SiC composite, manufactured during two separate time periods (9/99 and 1/01), were determined at 1038 and 1204 C by conducting tensile tests on specimens machined from plates. Continuous cycling fatigue tests (R = 0.05) and 20 cpm) were also conducted at the same two temperatures on specimens from both composites. In this study, average tensile properties, 95% confidence intervals associated with the tensile properties, and geometric mean fatigue lives of both composite materials are compared. The observed similarities and differences in the tensile properties are highlighted and an attempt is made to understand the relationship, if any, between the tensile properties and the fatigue behaviors of the two woven composites.

Kalluri, Sreeramesh↗
NASA NTRS2001

Creep/Rupture Behavior of Melt-Infiltrated SiC/SiC Composites Being Investigated

The failure behavior of melt-infiltrated SiC/SiC ceramic matrix composites is under investigation at the NASA Glenn Research Center as part of NASA's Ultra-Efficient Engine Technology Program. This material was originally developed under the High Speed Research Office's Enabling Propulsion Materials Program. Creep and rupture data provide accelerated testing information to predict material behavior under engine use situations (1500 to 2400 F). This information gives insights into various material development paths to improve composites as well as improve understanding of failure mechanisms. The left figure shows the fracture surface of a CMC material following over 200 hr of testing at 2400 F. This surface demonstrates the kind of fibrous pullout desirable for maximum crack deflection, hence non-brittle failure. Microscopy suggests that creep and rupture of these materials can best be considered as a probabilistic property, rather than a material property. Fiber failure occurs first in isolated regions, while stronger adjacent fibers remain intact. The right figure shows a region where oxide deposits blur and round the fiber images. Because the oxidation kinetics of SiC are well understood, this oxide scale can be used as a measure of the length of time various regions of the composites have been exposed to the environment, hence providing vital information regarding the sequence of failure. The oxide scale in the right figure indicates an early failure of this tow of fibers, whereas adjacent tows remain oxide free, suggesting failure much later in time. The path of various cracks can be followed throughout the composite in this manner, suggesting failure mechanisms.

Hurst, Janet B.↗
NASA NTRS2004

Durability and Design Issues of Thermal/environmental Barrier Coatings on Sic/sic Ceramic Matrix Composites Under 1650 C Test Conditions

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.

Zhu, Dong-Ming↗
NASA NTRS2003

Delamination Mechanisms of Thermal and Environmental Barrier Coatings on SiC/SiC Ceramic Matrix Composites

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.

Zhu, Dongming↗