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Advanced Woven SiC/SiC Composites for High Temperature Applications

The temperature, stress, and environmental conditions of many gas turbine, hypersonic, and even nuclear applications make the use of woven SiC/SiC composites an attractive enabling material system. The development in SiC/SiC composites over the past few years has resulted in significant advances in high temperature performance so that now these materials are being pursued for several turbine airfoil and reusable hypersonic applications. The keys to maximizing stress capability and maximizing temperature capability will be outlined for SiC/SiC. These include the type of SiC fiber, the fiber-architecture, and the matrix processing approach which leads to a variety of matrix compositions and structure. It will also be shown that a range of mechanical, thermal, and permeability properties can be attained and tailored depending on the needs of an application. Finally, some of the remaining challenges will be discussed in order for the use of these composite systems to be fully realized.

Morscher, Gregory N.↗

Evaluation of CVI SiC/SiC Composites for High Temperature Applications

Silicon carbide fiber reinforced silicon carbide (SiC/SiC) composites are candidate materials for various high temperature turbine engine applications because of their high specific strength and good creep resistance at temperatures of 1400 C (2552 F) and higher. Chemical vapor infiltration (CVI) SiC/SiC ceramic matrix composites (CMC) incorporating Sylramic-iBN SiC fiber were evaluated via fast fracture tensile tests (acoustic emission damage characterization to assess cracking behavior), tensile creep testing, and microscopy. The results of this testing and observed material behavior degradation mechanisms are reviewed.

testing↗

Damage Characterization in SiC/SiC Composites using Electrical Resistance

SiC/SiC ceramic matrix composites (CMCs) under creep-rupture loading accumulate damage by means of local matrix cracks that typically form near a stress concentration, such as a 90o fiber tow or large matrix pore, and grow over time. Such damage is difficult to detect through conventional techniques. Electrical resistance changes can be correlated with matrix cracking to provide a means of damage detection. Sylramic-iBN fiber-reinforced SiC composites with both melt infiltrated (MI) and chemical vapor infiltrated (CVI) matrix types are compared here. Results for both systems exhibit an increase in resistance prior to fracture, which can be detected either in situ or post-damage.

Smith, Craig E.↗

Constituent-Based Life Models Being Developed for SiC/SiC Composites

For the successful utilization of ceramic matrix composites (CMC) as hot-section components in advanced aeropropulsion engines, the CMC constituents will need to be tailored and optimized to meet all the critical property demands of each component. Under the High-Speed Research (HSR) and Advanced High-Temperature Engine Materials Technology (HITEMP) Programs, the NASA Glenn Research Center at Lewis Field initiated research to develop mechanistic models for key CMC thermostructural properties. These models would describe the effects of different constituent factors (composition, geometry, and volume fraction) and of potential application conditions (stress, time, temperature, and environment) on these properties. Particular focus was placed on both analytical and numerical modeling of state-of-the-art SiC/SiC composites where the primary load-bearing constituents are stoichiometric SiC fibers in a complex multiphase SiC matrix produced by chemical vapor infiltration and melt infiltration. Recent studies have resulted in computer-based numerical models for the elastic modulus, thermal expansion, and thermal conductivity properties of the SiC/SiC system. Additional studies have generated analytical and empirical models for the time dependence of composite rupture strength at temperatures above 2200 F (1200 C), where CMC's have an important thermostructural advantage over current nickel-based superalloys. These life models utilize thermal activation theory and fiber stress-rupture results measured at Glenn to generate Larson-Miller (L M) plots of fiber rupture strength versus q, a single time- and temperature-dependent parameter. Assuming a worse case in which the SiC matrix is cracked, rupture is then controlled by the time-dependent fracture characteristics of the fiber bundles bridging the matrix cracks. With this as the controlling mechanism, one can then use simple composite theory and the fiber L M plots to predict CMC rupture strength versus the q parameter. The dashed line shows the predicted rupture strength of a SiC/SiC composite that is reinforced by a state-of-the-art stoichiometric SiC fiber. For the q parameter, time is in hours and temperature in degrees kelvin. To generate these predictions, a two-dimensional 0 /90 composite with approximately 16 percent fiber in the applied stress direction and an air test environment were assumed. As such, it is possible to compare the model predictions against limited stress-rupture data for this CMC as shown by the data points. The good agreement confirms the rupture model at least for the selected CMC and test conditions. Thus for this particular SiC/SiC composite, one can estimate a 1000-hr rupture strength of approximately 12 ksi at 2400 F (T = 1588 K and q = 39 700 K). At lower CMC application stresses, the SiC matrix is typically uncracked, so both the fiber and matrix constituents share the composite load. In this case, CMC rupture is controlled by the constituent with the longest rupture time based on the creep rate of the composite. Measured Monkman-Grant plots of rupture time versus creep rate for the two SiC constituents have been used to develop CMC life models for this important application condition. NASA and DOD are currently using this information to establish application and material goals for more advanced CMC's that can be used at even higher temperatures.

DiCarlo, James A.↗

InSitu SEM Investigation of Microstructural Damage Evolution and Strain Relaxation in a Melt Infiltrated SiC/SiC Composite

With CMC components poised to complete flight certification in turbine engines on commercial aircraft within the near future, there are many efforts within the aerospace community to model the mechanical and environmental degradation of CMCs. Direct observations of damage evolution are needed to support these modeling efforts and provide quantitative measures of damage parameters used in the various models. This study was performed to characterize the damage evolution during tensile loading of a melt infiltrated (MI) silicon carbide reinforced silicon carbide (SiC/SiC) composite. A SiC/SiC tensile coupon was loaded to a maximum global stress of 30 ksi in a tensile fixture within an SEM while observations were made at 5 ksi increments. Both traditional image analysis and DIC (digital image correlation) were used to quantify damage evolution. With the DIC analysis, microscale damage was observed at the fiber-matrix interfaces at stresses as low as 5 ksi. First matrix cracking took place between 20 and 25 ksi, accompanied by an observable relaxation in strain near matrix cracks. Matrix crack opening measurements at the maximum load ranged from 200 nm to 1.5 m. Crack opening along the fiber-matrix interface was also characterized as a function of load and angular position relative to the loading axis. This characterization was funded by NASA GRC and was performed to support NASA GRC modeling of SiC/SiC environmental degradation

testing↗

Electrical Resistance as a NDE Technique to Monitor Processing and Damage Accumulation in SiC/SiC Composites

Ceramic matrix composites are suitable for high temperature structural applications such as turbine airfoils and hypersonic thermal protection systems. The employment of these materials in such applications is limited by the ability to process components reliable and to accurately monitor and predict damage evolution that leads to failure under stressed-oxidation conditions. Current nondestructive methods such as ultrasound, x-ray, and thermal imaging are limited in their ability to quantify small scale, transverse, in-plane, matrix cracks developed over long-time creep and fatigue conditions. Electrical resistance of SiC/SiC composites is one technique that shows special promise towards this end. Since both the matrix and the fibers are conductive, changes in matrix or fiber properties should relate to changes in electrical conductivity along the length of a specimen or part. Initial efforts to quantify the electrical resistance of different fiber and different matrix SiC/SiC composites will be presented. Also, the effect of matrix cracking on electrical resistivity for several composite systems will be presented. The implications towards electrical resistance as a technique applied to composite processing, damage detection, and life-modeling will be discussed.

Smith, Craig↗

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.↗

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↗

Thermo-Mechanical Properties of SiC/SiC Composites with Hybrid CVI-PIP Matrices

For long term structural service, the upper temperature capability for slurry-cast melt infiltrated (MI) SiC/SiC composites is limited to approx. 1315 C because of silicon reaction with the SiC fibers. For applications requiring material temperatures in excess of 1315 C, alternate methods of manufacturing the SiC matrices without silicon are being investigated, such as a hybrid combination of CVI and PIP. In this study, stacked fabric plies of Sylramic i-BN SiC fibers were coated with a CVI BN interface layer followed by a partial CVI SiC matrix. The remaining porosity in the SiC/SiC preforms was then infiltrated with silicon carbide matrix by PIP. Thermo-mechanical property measurements indicate that these composites are stable to 1700 C in inert environments under no load conditions for 100 h and under load conditions to 1450 C in air for 300 h. The advantages, disadvantages, and potential of this composite system for high temperature applications will be discussed.

Bhatt, R. T.↗

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↗

Advances in SiC/SiC Composites for Aerospace Applications

In recent years, supported by a variety of materials development programs, NASA Glenn Research Center has significantly increased the thermostructural capability of SiC/SiC composite materials for high-temperature aerospace applications. These state-of-the-art advances have occurred in every key constituent of the composite: fiber, fiber coating, matrix, and environmental barrier coating, as well as processes for forming the fiber architectures needed for complex-shaped components such as turbine vanes for gas turbine engines. This presentation will briefly elaborate on the nature of these advances in terms of performance data and underlying mechanisms. Based on a list of first-order property goals for typical high-temperature applications, key data from a variety of laboratory tests are presented which demonstrate that the NASA-developed constituent materials and processes do indeed result in SiC/SiC systems with the desired thermal and structural capabilities. Remaining process and microstructural issues for further property enhancement are discussed, as well as on-going approaches at NASA to solve these issues. NASA efforts to develop physics-based property models that can be used not only for component design and life modeling, but also for constituent material and process improvement will also be discussed.

DiCarlo, James A.↗

Fracture Mechanisms For SiC Fibers And SiC/SiC Composites Under Stress-Rupture Conditions at High Temperatures

The successful application of SiC/SiC ceramic matrix composites as high-temperature structural materials depends strongly on maximizing the fracture or rupture life of the load-bearing fiber and matrix constituents. Using high-temperature data measured under stress-rupture test conditions, this study examines in a mechanistic manner the effects of various intrinsic and extrinsic factors on the creep and fracture behavior of a variety of SiC fiber types. It is shown that although some fiber types fracture during a large primary creep stage, the fiber creep rate just prior to fracture plays a key role in determining fiber rupture time (Monkman-Grant theory). If it is assumed that SiC matrices rupture in a similar manner as fibers with the same microstructures, one can develop simple mechanistic models to analyze and optimize the stress-rupture behavior of SiC/SiC composites for applied stresses that are initially below matrix cracking.

DiCarlo, James A.↗

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.↗

In-Plane Cracking Behavior and Ultimate Strength for 2D Woven and Braided Melt-Infiltrated SiC/SiC Composites Tensile Loaded in Off-Axis Fiber Directions

The tensile mechanical properties of ceramic matrix composites (CMC) in directions off the primary axes of the reinforcing fibers are important for architectural design of CMC components that are subjected to multi-axial stress states. In this study, 2D-woven melt-infiltrated (MI) SiC/SiC composite panels with balanced fiber content in the 0 degree and 90 degree directions were tensile loaded in-plane in the 0 degree direction and at 45 degree to this direction. In addition, a 2D triaxially-braided MI composite panel with balanced fiber content in the plus or minus 67 degree bias directions and reduced fiber content in the axial direction was tensile loaded perpendicular to the axial direction tows (i.e., 23 degrees from the bias fibers). Stress-strain behavior, acoustic emission, and optical microscopy were used to quantify stress-dependent matrix cracking and ultimate strength in the panels. It was observed that both off-axis loaded panels displayed higher composite onset stresses for through-thickness matrix cracking than the 2D-woven 0/90 panels loaded in the primary 0 degree direction. These improvements for off-axis cracking strength can in part be attributed to higher effective fiber fractions in the loading direction, which in turn reduces internal stresses on critical matrix flaws for a given composite stress. Also for the 0/90 panel loaded in the 45 degree direction, an improved distribution of matrix flaws existed due to the absence of fiber tows perpendicular to the loading direction. In addition, for the +67/0/-67 braided panel, the axial tows perpendicular to the loading direction were not only low in volume fraction, but were also were well separated from one another. Both off-axis oriented panels also showed relatively good ultimate tensile strength when compared to other off-axis oriented composites in the literature, both on an absolute strength basis as well as when normalized by the average fiber strength within the composites. Initial implications are discussed for constituent and architecture design to improve the directional cracking of SiC/SiC CMC components with MI matrices.

Morscher, Gregory N.↗

Foreign Object Damage Behavior of a SiC/SiC Composite at Ambient and Elevated Temperatures

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.

Bhatt, Ramakrishna T.↗

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.↗

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.↗

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↗