Tensile creep properties and damage mechanisms of 2D-SiCf/SiC composites reinforced with low-oxygen high-carbon type SiC fiber

Tensile creep properties of 2D-SiC_f/SiC composites reinforced with low-oxygen high-carbon type SiC fibers were studied in vacuum at 1300°C∼1430°C. The fracture morphology was observed by scanning electron microscopy and the damage of fiber in 2D-SiC_f/SiC composites was characterized by nanoindentation. Moreover, the microstructure of the composite was investigated by high-resolution transmission electron microscopy. The results show that rupture time is much shortened and steady-state creep rate increase three orders of magnitude when creep temperature is higher than 1400°C. There are two different creep damage mechanisms due to the decrease of interfacial bonding strength at high temperature. The amorphous SiO_xC_y phase in the fibers can crystallize into SiC and C and the SiC grain grows in the fiber. The microstructural changes lead to the decrease of fiber strength and degrade the creep properties of the composite above 1400°C.     

Compressive creep of SiC whisker/Ti3SiC2 composites at high temperature in air

The compressive creep of a SiC whisker (SiC_w) reinforced Ti₃SiC₂ MAX phase-based ceramic matrix composites (CMCs) was studied in the temperature range 1100-1300°C in air for a stress range 20-120 MPa. Ti₃SiC₂ containing 0, 10, and 20 vol% of SiC_w was sintered by spark plasma sintering (SPS) for subsequent creep tests. The creep rate of Ti₃SiC₂ decreased by around two orders of magnitude with every additional 10 vol% of SiC_w. The main creep mechanisms of monolithic Ti₃SiC₂ and the 10% CMCs appeared to be the same, whereas for the 20% material, a different mechanism is indicated by changes in stress exponents. The creep rates of 20% composites tend to converge to that of 10% at higher stress. Viscoplastic and viscoelastic creep is believed to be the deformation mechanism for the CMCs, whereas monolithic Ti₃SiC₂ might have undergone only dislocation-based deformation. The rate controlling creep is believed to be dislocation based for all the materials which is also supported by similar activation energies in the range 650-700 kJ/mol.     

Tensile creep behavior of SiCf/SiC ceramic matrix minicomposites

Single fiber-tow minicomposites represent the major load-bearing element of woven and laminate ceramic matrix composites (CMCs). To understand the effects of fiber type, fiber content, and matrix cracking on tensile creep in SiC_f/SiC CMCs, single-tow SiC_f/SiC minicomposites with different fiber types and contents were investigated. The minicomposites studied contained either Hi-Nicalon™ or Hi-Nicalon™ Type S SiC fibers with a boron nitride (BN) interphase and a chemical-vapor-infiltrated-silicon-carbide (CVI-SiC) matrix. Tensile creep was performed at 1200 °C in air. A bottom-up creep modeling approach was applied where creep parameters of the fibers and matrix were obtained separately at 1200 °C. Next, a theoretical model based on the rule of mixtures was derived to model the fiber and matrix creep-time-dependent stress redistribution. Fiber and matrix creep parameters, load transfer model results, and numerical modeling were used to construct a creep strain model to predict creep damage evolution of minicomposites with different fiber types and contents.     

先驱体制备SiC纤维的发展历程与研究进展

碳化硅(SiC)纤维具有高强度、高模量、耐高温、抗蠕变、抗氧化等优异性能,是增强耐高温陶瓷基复合材料的关键材料。介绍了先驱体法制备3代SiC纤维的发展历程:从第1代高氧碳含量SiC纤维发展到第2代低氧高碳含量SiC纤维,再到第3代近化学计量比SiC纤维,SiC纤维的微结构从非晶到微晶显著变化,纤维的耐热性能也显著提高。重点比较了第3代近化学计量比SiC纤维(Hi-Nicalon Type S纤维、Tyranno SA和Sylramic纤维等)的性质,结果表明:SiC纤维的热稳定性由近化学计量比SiC微晶的致密度和微结构决定,Sylramic和Tyranno SA纤维的组成和微结构可通过控制Si-C-O纤维的碳热还原反应来实现,烧结助剂的采用及陶瓷烧结工艺的有效应用可提高纤维的致密度。Hi-Nicalon Type S纤维的组成和微结构取决于聚碳硅烷分解过程中特定的气氛和温度。简介了SiC纤维的研究进展并讨论了其发展趋势。     

Microstructure and tensile behavior of (BN/SiC)n coated SiC fibers and SiC/SiC minicomposites

Interphase plays an important role in the mechanical behavior of SiC/SiC ceramic-matrix composites (CMCs). In this paper, the microstructure and tensile behavior of multilayered (BN/SiC)_n coated SiC fiber and SiC/SiC minicomposites were investigated. The surface roughness of the original SiC fiber and SiC fiber deposited with multilayered (BN/SiC), (BN/SiC)₂, and (BN/SiC)₄ (BN/SiC)₈ interphase was analyzed through the scanning electronic microscope (SEM) and atomic force microscope (AFM) and X-ray diffraction (XRD) analysis. Monotonic tensile experiments were conducted for original SiC fiber, SiC fiber with different multilayered (BN/SiC)_n interfaces, and SiC/SiC minicomposites. Considering multiple damage mechanisms, e.g., matrix cracking, interface debonding, and fibers failure, a damage-based micromechanical constitutive model was developed to predict the tensile stress-strain response curves. Multiple damage parameters (e.g., matrix cracking stress, saturation matrix crack stress, tensile strength and failure strain, and composite’s tangent modulus) were used to characterize the tensile damage behavior in SiC/SiC minicomposites. Effects of multilayered interphase on the interface shear stress, fiber characteristic strength, tensile damage and fracture behavior, and strength distribution in SiC/SiC minicomposites were analyzed. The deposited multilayered (BN/SiC)_n interphase protected the SiC fiber and increased the interface shear stress, fiber characteristic strength, leading to the higher matrix cracking stress, saturation matrix cracking stress, tensile strength and fracture strain.     

Microstructural,strength, and creep characterization of Sylramic™, Sylramic™-iBN and super Sylramic™-iBN SiC fibers

The chemical composition, microstructure, strength, and thermal stability of polymer-derived Sylramic? SiC fibers fabricated by Dow Corning and COI Ceramics, Inc., and nitrogen-treated Sylramic? SiC fibers, referred to as Sylramic?-iBN and Super Sylramic?-iBN SiC fibers, were investigated and compared. The baseline Sylramic? SiC fibers fabricated by both vendors as well as the nitrogen-treated Sylramic? SiC fibers are composed mostly of β-SiC (～97 wt%) with small amounts of TiB₂ (～2 wt%), amorphous carbon (～1 wt%) and trace amounts of B₄C. Most of the amorphous carbon is segregated at the core/interior of the fibers. Both baseline and nitrogen-treated Sylramic? SiC fibers have similar grain size and pore size distribution, except for a thin layer of in-situ grown crystalline BN (30–70 nm) on the surface of Sylramic?-iBN and Super Sylramic?-iBN fibers. Wide variation in strength within a batch as well as between batches is observed in both baseline and nitrogen-treated Sylramic? SiC fibers but both types of fibers are microstructurally stable at temperatures to 1800 °C in argon and nitrogen environments compared to Nicalon?-S and Tyranno®-SA SiC fibers. Under the same creep condition, Super Sylramic?-iBN fibers show better creep resistance compared to Sylramic?, Sylramic?-iBN, Hi-Nicalon?-S, and Tyranno®-SA fibers. Possible reasons for strength variability and the mechanism of in-situ BN formation on Sylramic? SiC fibers are discussed.     

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.     

Relationship between microstructure and electromagnetic properties of SiC fibers

The microstructure and electromagnetic (EM) properties of four kinds of SiC fibers have been studied. These fibers are composed of amorphous SiC_xO_y, SiC nanocrystallines, free carbon, and nanopores, whose volume fractions are analyzed quantitatively. The content of free carbon notably affects the fiber's conductivity: the logarithm of conductivity increases linearly with the increase in the free carbon content when the volume fraction sum of free carbon and SiC exceed the percolation threshold. The EM loss mechanism is mainly composed of the conduction loss caused by free carbon and the polarization loss caused by SiC nanocrystallines. The content of free carbon is the decisive factor for the type of EM loss mechanism: the proportion of conduction loss increases linearly with the increase in free carbon content. Conduction loss is necessary for good EM absorption property, and polarization loss favors broadband absorption. For SiC fibers dominated by polarization loss, excellent absorption properties can be obtained in composites with higher fiber volume fraction (>20 vol%), which is crucial for structural absorbing materials.     

Micromechanical model of time-dependent damage and deformation behavior for an orthogonal 3D-woven SiC/SiC composite at elevated temperature in vacuum

This paper presents a micromechanical model to predict the time-dependent damage and deformation behavior of an orthogonal 3-D woven SiC fiber/BN interface/SiC matrix composite under constant tensile loading at elevated temperature in vacuum. In-situ observation under monotonic tensile loading at room temperature, load–unload tensile testing at 1200 °C in argon, and constant load tensile testing at 1200 °C in vacuum were conducted to investigate the effects of microscopic damage on deformation behavior. The experimentally obtained results led to production of a time-dependent nonlinear stress–strain response model for the orthogonal 3-D woven SiC/SiC. It was established using the linear viscoelastic model, micro-damage propagation model, and a shear-lag model. The predicted creep deformation was found to agree well with the experimentally obtained results.     

Creep of directionally solidified alumina/YAG eutectic monofilaments

Multi-phase—single crystal oxide fibers offer the best choice for reinforcing oxide matrix composites because they have superior creep resistance up to 1700 °C without significant strength loss at moderate temperatures due to growth of processing flaws. In this work, Directionally Solidified Al₂O₃–YAG eutectic fibers were grown at various rates by the Edge-defined, Film-fed Growth (EFG) method and their microstructure, microstructural stability and creep properties were studied. A methodology was developed in order to determine if the creep behavior of a fiber was affected by any heterogeneous coarsening defects. The creep behavior could be rationalized using a threshold stress concept with activation energy of 1100 kJ/mol K. TEM analysis of the crept fibers suggested that the Sapphire phase was deforming by a dislocation mechanism, while the YAG phase deformed by a diffusional mechanism. A creep model was developed which contained geometrical factors for describing the microstructure. Analysis of the data showed that the creep resistance would increase to single crystal values as the phase aspect ratio increased. Further, these two phases—single crystal structures exhibit a flaw-independent strength and are suggested to have a decrease in slow crack growth rate as the transverse phase size decreases.     

Mechanical properties and microstructural evolution of Cansas-III SiC fibers after thermal exposure in different atmospheres

Cansas-III SiC fibers were exposed in argon, air and wet oxygen (12%H₂O+8%O₂+80%Ar) atmospheres for 1 h at 1000–1500 °C. The pristine fiber consisted of β-SiC, free carbon and SiC_xO_y phases. After exposure in air and wet oxygen, an amorphous SiO₂ layer with embedding α-cristobalite crystals formed, while stacking faults were generated in the SiC core to release the residual stress. With the increasing oxidation temperature, lots of pores formed in the oxide layer, accompanied with the thickening, cracking and spallation of oxide layer. The average tensile strength decreased with the exposure temperature increasing and the exposure atmosphere deteriorating (argon→air→wet oxygen). After exposure at 1400 °C in argon and air, the fiber strength retention rates were 84% and 70%, respectively. However, after exposure at 1300 °C in wet oxygen, the strength retention rate was only 51%, indicating the accelerating oxidation and severe strength degradation of fibers.     

High-Temperature Creep and Microstructural Evolution of Chemically Vapor-Deposited Silicon Carbide Fibers

The creep behavior of three types of silicon carbide fibers that have been fabricated via chemical vapor deposition is described. The fibers exhibit only primary creep over the range of conditions studied (1200°–1400°C, 190–500 MPa). A transmission electron microscopy study of the microstructural development that is induced by the creep deformation of SCS-6 silicon carbide fibers at 1400°C is presented. Significant grain growth occurs in all silicon carbide regions of the fiber during creep, in contrast to the reasonably stable microstructure that is observed after annealing at the same temperature and time.     

Dynamic oxidation mechanism of SiC fiber reinforced SiC matrix composite in high-enthalpy plasmas

A plasma wind tunnel was utilized to explore the dynamic oxidation mechanism of SiC fiber reinforced SiC matrix composite in high-enthalpy plasmas. The results suggest the occurrences of active and passive oxidations on SiC fiber/matrix with atomic oxygen at 900～1600 °C and 1～6 kPa. Increasing plasma pressure could retard the active oxidation and promote the passive oxidation. Severe corrosion of SiC fibers due to active oxidation is highlighted. The as-formed SiO₂ layers cannot fully seal the open porosities and the interfacial gaps formed by oxidation of pyrocarbon interphases. This led to penetration of oxidized species and failure of fiber bundles directly exposed to heat flows. In addition, the spatial heat flux and temperature distributions were not homogeneous on the oxidized surface, which triggered early ‘temperature jump’ at ≈1600 °C (≈4.5 kPa) and severe localized ablation. If sealing the composite surface with SiC coating, the ablation resistance was significantly improved.     

SiC/SiC mini-composites with yttrium disilicate fiber coatings: Oxidation in steam

Solutions of YPO₄ were used to precipitate YPO₄ on pre-oxidized Hi-Nicalon-S SiC fibers. Tows of the coated fibers were then infiltrated with a preceramic polymer loaded with SiC particles to form mini-composites. During pyrolysis of the matrix, SiO₂ and YPO₄ on the fibers reacted and formed a Y₂Si₂O₇ fiber matrix interphase. Mini-composites were exposed to steam at 1000 °C for 10, 50, and 100 h, tensile tested, and the effect of oxidation in steam on the functionality of the Y₂Si₂O₇ fiber coating was investigated. The minicomposites oxidized at 1000 °C for 10 h retained 100 % of their unoxidized strength, and those oxidized for 50 and 100 h retained 92 % and 90 % of unoxidized strength, respectively. Strength retention and fiber pullout in both unoxidized and oxidized minicomposites suggests that the Y₂Si₂O₇ interphase was effective in maintaining a weak fiber-matrix interface.     

Oxidation of SiC/BN/SiC ceramic matrix composites in dry and wet oxygen at intermediate temperatures

The oxidation behavior of SiC/BN/SiC ceramic matrix composites (CMCs) was evaluated from 400° to 800 °C in 100% O₂ and 50% H₂O/50% O₂ gas mixtures. Thermogravimetric analysis (TGA) was utilized to measure weight change during controlled environment exposures at elevated temperatures for 1 and 50 hours. Oxidized CMCs and their oxides were studied post-exposure with scanning electron microscopy and energy dispersive spectroscopy. The oxidation onset and composition transition temperatures were evaluated. Key observations include oxide composition, oxide wetting, oxygen solubility in Hi-Nicalon SiC fibers and BN fiber coating oxidation and volatility behavior as a function of temperature. Degradation in wet environments at 600 °C was most extensive due to the formation of a non-wetting, non-protective surface oxide, allowing oxidant access to the BN fiber coatings followed by oxidation and volatilization. Implications of the CMC oxidation behavior are discussed for CMCs in service.     

Strength degradation of SiC fibers with a porous ZrB2-SiC coating: Role of the coating porous structure

ZrB₂-SiC coatings with varied porous structures were deposited on SiC fiber tows using the sol-gel method and cured at 1400 ℃ in vacuum. Tensile strength of the coated SiC fibers were much lower than that of the uncoated fibers. The bimodal distribution in the Weibull plot of the coated SiC fibers demonstrated that the fracture of the coated fiber can be attributed to two types of defects: the porous structure of the coating and the fiber defects. Detailed morphology and microstructure characterization of the coating and fiber combined with strength calculation were carried out to investigate the individual contribution of the fiber defects and the porous coating layer respectively. The results revealed that apart from the fiber damage during the coating process the porous structure of the fiber coating has a non-negligible effect on the fiber strength, presumably due to a relatively strong bonding between the fiber and coating.     

Wet chemical deposition of BN,SiC and Si3N4 interphases on SiC fibers

Fiber coatings based on BN, BN/SiC and BN/Si₃N₄ were deposited on Hi Nicalon type S SiC fibers. The coating parameters were optimized using a design of experiments study. With optimized parameter sets, the coatings exhibited a high degree of coverage on the fibers and almost no fiber bridging could be observed. The coated fiber bundles are flexible and can be processed further by techniques such as filament winding. In comparison to a non-processed reference sample, the maximum tensile load of the fiber bundles with BN, BN/SiC and BN/Si₃N₄ coatings was reduced by only 5 %, 13 % and 10 %, respectively. The coated fiber bundles retained their tensile strength after thermal annealing up to 1650 °C in a nitrogen atmosphere for 0.5 h. SiC_f/SiC samples with BN/SiC fiber coatings exhibited higher values of bending strength and strain-to-failure as a reference sample without fiber coating indicating the functionality of the fiber coatings.     

Evolution of microstructure and tensile strength of Cansas-II SiC fibers under air oxidizing atmosphere

The influence of oxidation on the microstructure and tensile strength of Cansas-II SiC fibers at 900–1500 ℃ in the air was investigated in depth. The growth of β-SiC grains ordering as well as the increase of the size of free carbon in the SiC core occurred due to the thermal exposure. The thickness of the amorphous SiO₂ layer increases with the temperature, starting to transform to cristobalite at 1200 ℃. The activation energy in the ambient air is determined as 148KJ/mol, similar to that of Hi-Niaclon fibers (107∼151 KJ/mol). With the growth of the SiO₂ layer, lots of bubbles appeared in the SiO₂ layer due to the release of excess CO gas. Moreover, many cracks occurred on the fiber surface caused by the residual stress. The mean tensile strength decreased from initial 2.7 GPa to 0.3 GPa after the treatment at 1500 ℃, which could be mainly attributed to the SiO₂ layer.     

Interaction of fiber matrix bonding in SiC/SiC ceramic matrix composites

Non-oxide ceramic matrix composites (CMC) based on SiC fibers with SiC matrix were fabricated by polymer infiltration and pyrolysis (PIP) and characterized regarding their microstructural features and their mechanical properties. The fiber preform was made using winding technology. During the winding process, the SiC fiber roving was impregnated by a slurry containing SiC powder and sintering additives (Y₂O_3, Al₂O₃ and SiO₂). This already helped to achieve a partial matrix formation during the preform fabrication. In this way, the number of PIP cycles to achieve composites with less than 10% open porosity could be reduced significantly. Additionally, damage-tolerant properties of the composites were obtained by an optimal design of the matrix properties although only uncoated fibers were used. Finally, composites with a strength level of about 500 MPa and a damage-tolerant fracture behavior with about 0.4% strain to failure were obtained.     

Study of SiC fiber axial compressive behavior using tensile recoil measurement

SiC fibers have been widely investigated as reinforcements for advanced ceramic matrix composites owing to their excellent high-temperature properties. However, the axial compressive strength of SiC fibers has not been thoroughly studied. In this study, the compressive behavior of two SiC fiber types containing different compositions and thermal degradation were characterized by tensile recoil measurements. Results illustrated that the SiC fiber compressive strength was 30%–50% of its tensile strength, after heat treatment at 1200℃–1800℃ for 0.5 h in argon. The fiber compressive failure mechanism was studied, and a “shear-bending-cleavage” model was proposed for the recoil compression fracture of pristine SiC fibers. The average compressive and tensile strengths of the pristine SiC-II fiber were 1.37 and 3.08 GPa, respectively. After treatment at 1800℃ for 0.5 h in argon, the SiC-II fiber compressive strength decreased to 0.42 GPa, whereas the tensile strength reduced to 1.47 GPa. The mechanical properties of the fibers degraded after high-temperature treatment. This could be attributed to SiC grain coarsening and SiC_xO_y phase decomposition.