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

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

Chulya, Abhisak↗

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

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

Morscher, G. N.↗

Characterizing the Properties of a Woven SiC/SiC Composite Using W-CEMCAN Computer Code

A micromechanics based computer code to predict the thermal and mechanical properties of woven ceramic matrix composites (CMC) is developed. This computer code, W-CEMCAN (Woven CEramic Matrix Composites ANalyzer), predicts the properties of two-dimensional woven CMC at any temperature and takes into account various constituent geometries and volume fractions. This computer code is used to predict the thermal and mechanical properties of an advanced CMC composed of 0/90 five-harness (5 HS) Sylramic fiber which had been chemically vapor infiltrated (CVI) with boron nitride (BN) and SiC interphase coatings and melt-infiltrated (MI) with SiC. The predictions, based on the bulk constituent properties from the literature, are compared with measured experimental data. Based on the comparison. improved or calibrated properties for the constituent materials are then developed for use by material developers/designers. The computer code is then used to predict the properties of a composite with the same constituents but with different fiber volume fractions. The predictions are compared with measured data and a good agreement is achieved.

Murthy, Pappu L. N.↗

Design, Fabrication, and Testing of Ceramic Joints for High Temperature SiC/SiC Composites

Various issues associated with the design and mechanical evaluation of joints of ceramic matrix composites are discussed. The specific case of an affordable, robust ceramic joining technology (ARCJoinT) to join silicon carbide (CG-Nicalon(sup TM)) fiber-reinforced-chemically vapor infiltrated (CVI) silicon carbide matrix composites is addressed. Experimental results are presented for the time and temperature dependence of the shear strength of these joints in air up to 1200 C. From compression testing of double-notched joint specimens with a notch separation of 4 mm, it was found that the apparent shear strength of the joints decreased from 92 MPa at room temperature to 71 MPa at 1200 C. From shear stress-rupture testing in air at 1200 C it was found that the shear strength of the joints decreased rapidly with time from an initial shear strength of 71 to 17.5 MPa after 14.3 hr. The implications of these results in relation to the expected long-term service life of these joints in applications at elevated temperatures are discussed.

Singh, Mrityunjay↗

Growth of Matrix Cracks During Intermediate Temperature Stress Rupture of a SiC/SiC Composite in Air

The crack density of woven Hi-Nicalon(sup TM) (Nippon Carbon, Japan) fiber, BN interphase, melt-infiltrated SiC matrix composites was determined for specimens subjected to tensile stress rupture at 815 C. A significant amount of matrix cracking occurs due to the growth of fiber-bridged microcracks even at stresses below the run-out condition. This increased cracking corresponded to time dependent strain accumulation and acoustic emission activity during the constant load test. However, the portion of the rupture specimens subjected to cooler temperatures (< 600 C than the hot section had significantly lower crack densities compared to the hotter regions. From the acoustic emission and time dependent strain data it can be inferred that most of the matrix crack growth occurred within the first few hours of the tensile rupture experiment. The crack growth was attributed to an interphase recession mechanism that is enhanced by the presence of a thin carbon layer between the fiber and the matrix as a result of the composite fabrication process. One important consequence of matrix crack growth at the lower stresses is poor retained strength at room temperature for specimens that did not fail.

Morscher, Gregory N.↗

Mechanical Behavior of Notched SiC/SiC Composites

Gas turbine components such as combustor liners or turbine vanes are subject to regions of high stress-concentration, e.g., attachment to the frame or at cooling holes. Ceramic matrix composites (CMCs) are potential materials for high temperature applications in gas turbines. They offer some capability to relieve stress at regions of high stress-concentration via matrix damage accumulation. In this study notch sensitivity was examined for woven SiC fiber reinforced, melt-infiltrated SiC matrix composites with a BN interphase, utilizing either Hi-Nicalo(TM) fibers or the stiffer Sylramic fibers. The double-edge notched tensile test approach was used for a wide range of notch sizes and specimen widths. Both composite systems exhibited mild notch sensitivity similar to other CMC systems. Acoustic emission, detected during the tensile tests, indicated that matrix cracking occurred around notches at net-section stresses below the stress where matrix cracking first occurs in unnotched specimens. However, thermoelastic stress analysis did not show any measurable stress relief around notches after the specimens were preloaded.

Morscher, Gregory N.↗

Room Temperature Creep Of SiC/SiC Composites

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

Morscher, Gregory N.↗

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

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

Morscher, Gregory N.↗

C-Coupon Studies of SiC/SiC Composites: Microstructual Characterization - Part 2

A 'C-coupon' was used to measure the interlaminar tensile behavior of five different composite materials: Sylramic/MI (melt infiltration SiC matrix), ZMl/MI, Sylramic/S300, and ZMI and Hi-Nicalon with an S200 matrix at room temperature, 816 C, and 1204 C. Fracture behavior was characterized by field emission scanning electron microscopy, and observed cracking compared with events measured by modal acoustic emission. Both radial and matrix hoop cracking along the inner radius arising from hoop stresses were observed for all material types. In those composites in which the radial cracks were sufficiently wide to view the composite interior, fracture was observed to occur at the fiber BN or BN matrix interface.

Hurwitz, Frances I.↗

Intermediate Temperature Strength Degradation in SiC/SiC Composites

Woven silicon carbide fiber-reinforced, silicon carbide matrix composites are leading candidate materials for an advanced jet engine combustor liner application. Although the use temperature in the hot region for this application is expected to exceed 1200 C, a potential life-limiting concern for this composite system exists at intermediate temperatures (800 +/- 200 C), where significant time-dependent strength degradation has been observed under stress-rupture loading. A number of factors control the degree of stress-rupture strength degradation, the major factor being the nature of the interphase separating the fiber and the matrix. BN interphases are superior to carbon interphases due to the slower oxidation kinetics of BN. A model for the intermediate temperature stress-rupture of SiC/BN/SiC composites is presented based on the observed mechanistic process that leads to strength degradation for the simple case of through-thickness matrix cracks. The approach taken has much in common with that used by Curtin and coworkers, for two different composite systems. The predictions of the model are in good agreement with the rupture data for stress-rupture of both precracked and as-produced composites. Also, three approaches that dramatically improve the intermediate temperature stress-rupture properties are described: Si-doped BN, fiber spreading, and 'outside debonding'.

Morscher, Gregory N.↗

The Velocity and Attenuation of Acoustic Emission Waves in SiC/SiC Composites Loaded in Tension

The behavior of acoustic waves produced by microfracture events and from pencil lead breaks was studied for two different silicon carbide fiber-reinforced silicon carbide matrix composites. The two composite systems both consisted of Hi-Nicalon (trademark) fibers and carbon interfaces but had different matrix compositions that led to considerable differences in damage accumulation and acoustic response. This behavior was primarily due to an order of magnitude difference in the interfacial shear stress for the two composite systems. Load/unload/reload tensile tests were performed and measurements were made over the entire stress range in order to determine the stress-dependence of acoustic activity for increasing damage states. It was found that using the extensional wave velocities from acoustic emission (AE) events produced from pencil lead breaks performed outside of the transducers enabled accurate measurements of the stiffness of the composite. The extensional wave velocities changed as a function of the damage state and the stress where the measurement was taken. Attenuation for AE waveforms from the pencil lead breaks occurred only for the composite possessing the lower interfacial shear stress and only at significantly high stresses. At zero stress after unloading from a peak stress, no attenuation occurred for this composite because of crack closure. For the high interfacial stress composite no attenuation was discernable at peak or zero stress over the entire stress-range of the composite. From these observations, it is believed that attenuation of AE waveforms is dependent on the magnitude of matrix crack opening.

Morscher, Gregory N.↗

Damage Accumulation in SiC/SiC Composites with 3D Architectures

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

Morscher, Gregory N.↗

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

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

Morscher, Gregory N.↗

SiC/SiC Composites for 1200 C and Above

The successful replacement of metal alloys by ceramic matrix composites (CMC) in high-temperature engine components will require the development of constituent materials and processes that can provide CMC systems with enhanced thermal capability along with the key thermostructural properties required for long-term component service. This chapter presents information concerning processes and properties for five silicon carbide (SiC) fiber-reinforced SiC matrix composite systems recently developed by NASA that can operate under mechanical loading and oxidizing conditions for hundreds of hours at 1204, 1315, and 1427 C, temperatures well above current metal capability. This advanced capability stems in large part from specific NASA-developed processes that significantly improve the creep-rupture and environmental resistance of the SiC fiber as well as the thermal conductivity, creep resistance, and intrinsic thermal stability of the SiC matrices.

DiCarlo, J. A.↗

Microstructural Optimization of High Temperature SiC/SiC Composites

Advanced materials and process approaches are described that have allowed NASA to develop five state-of-the-art silicon carbide (SiC) fiber-reinforced hybrid-SiC matrix composite systems that can operate under mechanical loading and oxidizing conditions for hundreds of hours at upper use temperatures from 1200 to 1450 C. Key data are presented that demonstrate the ability of these materials to meet the first-level property requirements for hot-section components in advanced gas turbine engines.

DiCarlo, James A.↗

Thermomechanical Fatigue Behavior of Coated and Uncoated Enhanced SiC/SiC Studied

Thermomechanical fatigue (TMF) testing provides a method of evaluating candidate continuous-fiber-reinforced ceramic composites under thermal and mechanical loading conditions. Although these tests are complicated, they provide a reasonable approximation of the combined thermal and mechanical loads that will be experienced by the material in service. The resulting data will be used to develop life-prediction models as well as to aid materials development.

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