Fatigue behavior and damage analysis of PIP C/SiC composite

In this work, we study the fatigue behavior of a C/SiC composite produced by several cycles of polymer infiltration and pyrolysis (PIP). Fatigue tests were performed with maximum stresses corresponding to 60–90% of the tensile strength of the composite. During the fatigue tests, acoustic emission (AE) monitoring was performed and the measured AE energy was utilized to quantify the damage and distinguish possible damage mechanisms. Most of the fatigue damage in the form of matrix cracking, interface damage and fiber breakage occurs in the first cycle. As loading cycles proceeded, damage in form of matrix crack re-opening and interfacial friction constantly accumulates. Nevertheless, all samples survived the run-out of 1,000,000 cycles. After the fatigue tests, an increase of the tensile strength is observed. This phenomenon is associated with the relief of process-induced internal thermal stresses and the weakening of the fiber-matrix interface. In general, the studied material shows very high relative fatigue limit of 90% of its tensile strength.     

Fatigue behaviour and residual strength evolution of 2D C/SiC Z-pinned joints prepared by chemical vapour infiltration

Z-pinned joints prepared by chemical vapour infiltration are widely used in ceramic matrix composite components. Excellent fatigue behaviour is important for structural safety. In this study, 2D C/SiC Z-pinned joints were loaded in axial direction of the pins under static and cyclic loading. Internal damage was monitored in situ by an acoustic emission system. The binding force between pin and hole is relatively strong. Meanwhile, the joints exhibite promising resistance to fatigue. The residual strength increased first with the fatigue cycles then decreased after 10⁵ cycles. Microstructural analysis indicated that full-developed cracks and local stress redistribution resultes in the increase in the strength of the joints. The acoustic emission analysis also provides a supplementary understanding of the damage mechanism. The results show that damage fully develops at the early stage of fatigue. When the specimen is reloaded, less AE events are collected before the fatigue maximum stress.     

Does a True Fatigue Limit Exist for Continuous Fiber-Reinforced Ceramic Matrix Composites?

The high-cycle high-frequency fatigue behavior of a Nicalon-fiber-reinforced calcium aluminosilicate ceramic composite was investigated. A key goal of the room-temperature fatigue experiments was to determine if a true fatigue limit or endurance limit existed for this ceramic matrix composite. Although no fatigue failures occurred beyond 10⁷ cycles, the stress–strain hysteresis modulus and frictional heating continued to change up to 10⁸ cycles, at which point the 200 Hz experiments were terminated. This suggests that fatigue damage continued to evolve and that a true fatigue limit may not exist in ceramic matrix composites that have undergone interfacial frictional sliding.     

Comparative Analysis of Low‐Cycle Fatigue Behavior of 2D‐Cf‐PyC/SiC Composites in Different Environments

A carbon fiber‐reinforced silicon carbide matrix composite with pyrolytic carbon interface (C_f‐PyC/SiC) and a protective coating was prepared by isothermal low pressure chemical vapor infiltration. Low‐cycle fatigue behavior of this material system was investigated at high temperatures up to 1800°C in a combustion environment and at room temperature in air, respectively. The combustion environment includes thermal mechanical loading, high temperatures, and oxidizing atmosphere. Low‐cycle fatigue tests were conducted at a maximum stress level of 180 MPa but at various temperatures and fatigue cycles. The residual strength variation of fatigue‐survived samples was due to different damage mechanisms in different environments.     

Modeling deformation of a melt-infiltrated SiC/SiC composite under fatigue loading

Results from fatigue experiments done on a SiC/SiC composite are presented. A micromechanics-based model is used to study the observed behavior under cyclic loading. The model includes consideration of progressive damage, creep and oxidation of the fiber and matrix. Comparison of model predictions with test data showed that the deformation during fatigue in this material is explained primarily by damage in the form of matrix microcracking and interface debonding, in combination with creep under the cyclic load. Stiffness of the material was observed to not change significantly during fatigue indicating that the contribution of fiber fracture to deformation is limited. Fiber fracture however was found to determine final failure of the composite. Failure under cyclic fatigue loading was found to be affected by load transfer from the matrix to the fiber due to damage and creep, and by progressive degradation of the load-carrying fibers due to the combined effect of oxidation and load cycling.     

Fatigue of three advanced SiC/SiC ceramic matrix composites at 1200°C in air and in steam

High‐temperature mechanical properties and tension‐tension fatigue behavior of three advanced SiC/SiC composites are discussed. The effects of steam on high‐temperature fatigue performance of the ceramic‐matrix composites are evaluated. The three composites consist of a SiC matrix reinforced with laminated, woven SiC (Hi‐Nicalon?) fibers. Composite 1 was processed by chemical vapor infiltration (CVI) of SiC into the Hi‐Nicalon? fiber preforms coated with boron nitride (BN) fiber coating. Composite 2 had an oxidation inhibited matrix consisting of alternating layers of silicon carbide and boron carbide and was also processed by CVI. Fiber preforms had pyrolytic carbon fiber coating with boron carbon overlay applied. Composite 3 had a melt‐infiltrated (MI) matrix consolidated by combining CVI‐SiC with SiC particulate slurry and molten silicon infiltration. Fiber preforms had a CVI BN fiber coating applied. Tensile stress‐strain behavior of the three composites was investigated and the tensile properties measured at 1200°C. Tension‐tension fatigue behavior was studied for fatigue stresses ranging from 80 to 160 MPa in air and from 60 to 140 MPa in steam. Fatigue run‐out was defined as 2 × 10⁵ cycles. Presence of steam significantly degraded the fatigue performance of the CVI SiC/SiC composite 1 and of the MI SiC/SiC composite 3, but had little influence on the fatigue performance of the SiC/SiC composite 2 with the oxidation inhibited matrix. The retained tensile properties of all specimens that achieved fatigue run‐out were characterized. Composite microstructure, as well as damage and failure mechanisms were investigated.     

Fatigue Damage Accumulation in 3-Dimensional SiC/SiC Composites

The effect of fatigue loading on the mechanical performance of 3-D SiC/SiC composites was investigated. A non-destructive macromechanical approach was applied which permits for the evaluation of the material damage state by monitoring its dynamic response as function of fatigue cycles. The correlation of the results provided by this method to that of other non-destructive techniques such as Acoustic Emission (AE), leads to a detail micromechanical-macromechanical monitoring of the material fatigue behaviour. The damage modes identification and their successive appearance, together with the evaluation of the material performance at the different stages of fatigue loading, is among the inspection capabilities that provides the above mentioned combination of non-destructive techniques. The proposed methodology applied in the case of a 3-D SiC/SiC ceramic matrix composite material and the effect of fatigue loading on the material integrity was evaluated by measuring the degradation of the dynamic modulus of elasticity and the increase of the material damping. Conclusions, concerning design aspects using these materials, as well as fatigue life prediction were provided. Finally, the sensitivity of the proposed methodology for the definition, the characterisation of the development and the separation of the different damage modes during fatigue loading has been discussed.     

High-Frequency Fatigue Behavior of Woven-Fiber-Fabric-Reinforced Polymer-Derived Ceramic-Matrix Composites

The monotonic and high-frequency (100 Hz) fatigue behavior of two Nicalon-fabric-reinforced SiCON matrix composites was investigated at room temperature. The matrix composition was varied by the addition of BN and SiC particulate fillers, to contain shrinkage from processing by polymer infiltration and pyrolysis (PIP). The composites had strong fiber/matrix bonding, which resulted in substantially less frictional heating than observed with weakly bonded composites. Both composites exhibited fatigue runout at 10⁷ cycles at ∼80% of the monotonic strength. Comparison with existing fatigue data in the literature (for the same composites) at 1 Hz shows no change in fatigue life; i.e., no frequency effect was observed. Most of the stiffness reduction in the composites occurred in the first fatigue cycle, whereas subsequent decreases in moduli were attributed to limited fiber cracking. The major driving force for failure was the localized debonding of transverse and longitudinal plies at the crossover points in the fabric, which, when linked, resulted in interlaminar damage and failure in the composite.     

Low-cycle fatigue behavior of flexible 3D printed thermoplastic polyurethane blends for thermal energy storage/release applications

Thermal energy storage (TES) materials constituted by a microencapsulated paraffin having a melting temperature of 6°C and a thermoplastic polyurethane (TPU) matrix were prepared through fused deposition modeling. Scanning electron microscope (SEM) micrographs demonstrated that the microcapsules were homogeneously distributed within the matrix, with a rather good adhesion within the layers of 3D printed specimens, even at elevated concentrations of microcapsules. The presence of paraffin capsules having a rigid polymer shell lead to a stiffness increase, associated to a decrease in the stress and in the strain at break. Tensile and compressive low-cycles fatigue tests showed that the presence of microcapsules negatively affected the fatigue resistance of the samples, and that the main part of the damage occurred in the first fatigue cycles. After the first 10 loading cycles at 50% of the stress at break, a decrease in the elastic modulus ranging from 60% for neat TPU to 80% for composite materials was detected. This decrease reached 40% of the original value at 90% of the stress at break after 10 cycles. Differential scanning calorimetry tests on specimens after fatigue loading highlighted a substantial retention of the original TES capability, in the range of 80%–90% of the pristine value, even after 1000 cycles, indicating that the integrity of the capsules was maintained and that the propagation of damage during fatigue tests took probably place within the surrounding polymer matrix. It could be therefore concluded that it is possible to apply the developed blends in applications where the materials are subjected to cyclic stresses, both in tensile and compressive mode.     

Fatigue behavior of continuous glass fiber composites: Effect of the matrix nature

The effect of the matrix morphology on the fatigue behavior of a continuous glass fiber/polypropylene (GF/PP) composite system was studied by means of stress‐life and mode II cyclic delamination tests. The stress‐life behavior of a GF composite is considerably affected by the nature of the matrix. A two‐stage fatigue damage curve was observed in the composite made with a PP matrix, whereas a three‐stage curve was observed in the composite made with a thermoset polyester matrix. For a fatigue stress higher than 50% of the yield stress, the PP matrix composite showed a considerably longer fatigue life than the thermoset polyester matrix composite. Mode II cyclic delamination tests showed that the morphology itself of the PP matrix also played an important role. Higher fatigue delamination growth rates, at given strain energy release rates, and lower strain energy release rates at failure were obtained for a composite showing a coarse spherulitic morphology and well‐marked interspherulitic regions than for a composite showing a finer spherulitic morphology and less‐marked interspherulitic regions. While the fatigue mode of the composite with a coarse spherulitic morphology was interspherulitic, that of the composite with a finer spherulitic morphology was transpherulitic.     

Experimental Observations of Frictional Heating in Fiber-Reinforced Ceramics

The influence of fatigue loading history and microstructural damage on the magnitude of frictional heating and interfacial shear stress in a unidirectional SiC fiber/calcium aluminosilicate matrix composite was investigated. The extent of frictional heating was found to depend upon loading frequency, stress range, and average matrix crack spacing. The temperature rise attained during fatigue can be significant. For example, the temperature rise exceeded 100 K during fatigue at 75 Hz between stress limits of 220 and 10 MPa. Analysis of the frictional heating data indicates that the interfacial shear stress undergoes an initially rapid decrease during the initial stages of fatigue loading: from an initial value over 20 MPa, to approximately 5 MPa after 25 000 cycles. Over the range of 5 to 25 Hz, the interfacial shear stress was not significantly influenced by loading frequency. The implications of frictional heating in fiber-reinforced ceramics are also discussed.     

Fatigue of a SiC/SiC ceramic composite with an ytterbium-disilicate environmental barrier coating at elevated temperature*

Tension-tension fatigue performance of a SiC/SiC composite with an ytterbium-disilicate environmental barrier coating (EBC) was investigated at 1200°C in air and steam. The composite is reinforced with Hi-Nicalon™ SiC fibers and has a melt-infiltrated matrix processed by chemical vapor infiltration of SiC with subsequent infiltration with SiC particulate slurry and molten silicon. The EBC consists of a Si bond coat and an Yb₂Si₂O₇ top coat applied via air plasma spraying. Tensile properties were evaluated at 1200°C. Tension-tension fatigue was examined for maximum stresses of 110-140 MPa. To assess the efficacy of EBC, experimental results obtained for the coated composite are compared to those for a control uncoated composite. Surface grit-blasting inherent in the EBC application process degrades tensile strength of the composite. However, the EBC effectively protects the composite from oxidation embrittlement during cyclic loading in air or steam. Fatigue runout set to 200 000 cycles (55.6 hours at a frequency of 1.0 Hz) was achieved at 110 MPa in air and steam. Retained properties of pre-fatigued specimens were characterized. Composite microstructure, along with damage and failure mechanisms were investigated. Damage and failure of the composite are attributed to the growth of cracks originating from numerous processing defects in the composite interior.     

Fatigue behavior and damage evolution of SiC/SiC composites under high-temperature anaerobic cyclic loading

In the present study, the fatigue behavior and damage evolution of SiC/SiC minicomposites at elevated temperatures in oxygen-free environment are investigated which are important for their application and are still unclear. The high-temperature fatigue test platform is developed and the fatigue stress-life curve and the stress-strain response are obtained. The test result shows that the life of the material at elevated temperature is shorter than that at room temperature under the same stress level. Moreover, the hysteresis loop width and the residual strain increase with the increasing of the cycles while the hysteresis modulus decreases during the fatigue cycling. The evolution process of matrix cracks is observed using the real-time remote detection system. It is found that matrix cracking is insensitive to the cyclic loading which is similar to room temperature and is due to that the degeneration of the interfacial shear stress reduces the area of high stress in matrix. The fiber/matrix interfacial shear stress under different cycles is determined based on the fatigue modulus of each hysteresis loop. The result shows a fatigue enhancement phenomenon for the interface which is not observed at room temperature.     

Rate of Strength Decrease of Fiber-Reinforced Ceramic-Matrix Composites during Fatigue

An experimental investigation was performed to study the rate at which strength-controlling fatigue damage evolves in a ceramic-matrix composite. Tensile specimens of a unidirectional SiC-fiber-reinforced calcium aluminosilicate matrix composite were cycled to failure or to a preselected number of cycles under similar loading histories. The residual strength of the precycled specimens was found to be similar to that of virgin specimens. Microstructural investigations showed that the fracture surfaces of the specimens cycled to failure had a central region where fiber pullout was negligible. It is proposed that frictional heating (due to interfacial sliding) is the cause of fatigue failure. High interfacial temperatures are assumed to cause the formation of a strong interface bond, leading to internal embrittlement.     

Tensile and fatigue behavior of oxide/oxide ceramic matrix composite with simulated foreign object damage in combustion environment

In this study, oxide/oxide ceramic matrix composite test coupons were quasi‐statically indented and tested for tensile strength and fatigue life in a combustion environment. The combustion environment simulated the gas turbine engine environment in an aircraft. Two different dent sizes were created on two different sets of test coupons with a blunt conical indentor. During mechanical testing, the combustion flame simultaneously impinged on the dent region resulting in a maximum test coupon surface temperature of 1250 ± 50°C. For a life of 90 000 cycles, the fatigue limit in the combustion environment was 85% of the postindentation degraded tensile strength. Microscopy images of the failed test coupons showed damage modes of fiber fracture and matrix cracking at the dent site. The run‐out test coupons which did not fail within 90 000 cycles showed residual strength that was not significantly different from that of their virgin counterparts.     

Tensile fatigue of a laminated carbon-carbon composite at room temperature

The tensile fatigue behavior of a cross-ply carbon-carbon (C/C) laminate was examined at room temperature. Tension-tension cyclic fatigue tests were conducted under load control at a sinusoidal frequency of 10 Hz to obtain stress-fracture cycles (S-N) relationship. The fatigue limit of the C/C was found to be 213 MPa (93% of the tensile strength), and no fracture was observed at over 10⁴ cycles. The residual tensile strength of specimens that survived fatigue loading was enhanced with increase in fatigue cycles and applied stress. Observations of the fatigue-loaded specimens revealed that the formation of micro-cracks at the fiber-matrix interfaces was facilitated during fatigue loading. These interfacial cracks were concluded to protect the fibers from being damaged by matrix cracks and this behavior was considered to be the governing mechanism of strength enhancement by fatigue loading.     

Fatigue resistance and damage mechanisms of 2D woven SiC/SiC composites at high temperatures

Fatigue resistance and damage mechanisms of 2D woven SiC/SiC composites at high temperatures were investigated in this research. Fatigue behavior tests were performed at 1200℃ and 1000°C at 10 Hz and stress ratio of 0.1 for maximum stresses ranging from 80 to 120 MPa, and the fatigue run-out could be defined as 10⁶ cycles. Evolution of the cumulative displacement and normalized modulus with cycles was analyzed for each fatigue condition. Fatigue run-out was achieved at 80 MPa and 1000°C. It could be found that the cycle lifetimes of the composites decreased sharply with the increasing maximum stress and temperature conditions significantly affected the fatigue performance under matrix cracking stress. The cumulative displacement showed no noticeable increase before 1000 cycles and the modulus of the failed specimens decreased before fracture. The retained properties of composites that achieved fatigue run-out, as well as the microstructures, were characterized in order to understand the fatigue behavior and failure mechanisms. The composites exhibited similar fracture morphology with matrix crack extension and glass phase oxidation formation under different conditions. In general, the high-temperature fatigue damage and failure of composites could be affected by combination of stress damage and oxidative embrittlement.     

Effect of oxidation on the bending fatigue behavior of an advanced SiC/SiC CMC component at 1000 °C in air

The present study elucidates the effect of oxidation during static and fatigue loading in SiC/SiC CMC structured component, which shows damage in the stress-concentrated region. It is made of Tyranno SA3 fiber, BN (Boron nitride) interphase, and CVI (chemical vapor infiltration) + PIP (polymer impregnation and pyrolysis) hybrid matrix. The comparison based on strength and fracture morphology was made. After annealing, the as-received sample showed minute oxidation and slightly enhanced strength. The fatigued sample without annealing under low stress showed higher retained strength than the as-received sample due to smooth debonding. The fatigued sample with annealing under high stress showed a loss in strength than the as-received sample owing to the formation of a significant amount of borosilicates glasses, which further promoted SiO₂ formation between fiber and matrix and caused the brittle failure. However, simultaneous filling borosilicate glasses into the pores oppositely aided in maintaining the retained strength.     

Tensile and Fatigue Behavior of Silicon Carbide Fiber-Reinforced Aluminosilicate Glass

The onset of damage accumulation in ceramic-matrix composites occurs as matrix microcracking and fiber/matrix debonding. Tension tests were used to determine the stress and strain levels to first initiate microcracking in both unidirectional and cross-ply laminates of silicon carbide fiber-reinforced aluminosilicate glass. Tension–tension fatigue tests were then conducted at stress levels below and above the matrix cracking stress level. At stress levels below matrix microcracking, no loss in stiffness occurred. At stresses above matrix cracking, the elastic modulus of the unidirectional specimens exhibited a gradual decrease during the first 10 000 cycles, and then stabilized. However, the cross-ply material sustained most of the damage on the first loading cycle. It is shown that fatigue life can be related to nonlinear stress–strain behavior of the 0° plies, and that the cyclic strain limit was approximately 0.3%.     

Influence of oxidation on fatigue life of a carbon/silicon carbide composite in water vapor containing environments

The influence of oxidation on the fatigue life of two-dimensional carbon/silicon carbide composites in water vapor containing environments at 1300 °C was investigated. Tension–tension fatigue experiments were conducted at sinusoidal frequency of 3 Hz. Using a stress ratio (σ_min/σ_max) of 0.1, specimens were subjected to peak fatigue stresses of 90, 120 and 150 MPa. The mean residual strength of the specimens after survived 100,000 cycles with a peak stress of 90 MPa was 83.9% of that of the as-received composite. The mean fatigue lives of the specimens subjected to peak fatigue stresses of 120 and 150 MPa were 42,048 and 13,514 cycles, respectively. Oxidation was the dominant damage mechanism, which remarkably decreased the fatigue life. Oxidizing species diffusion within the composite defects was discussed. The higher the applied stresses, the larger the equivalent radius of the defect and the shorter the fatigue life.