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.     

Matrix cracking of 2D SiC/SiC composite characterized by in situ SEM and nano-CT

Two-dimensional plain-woven silicon carbide (SiC) fiber-reinforced SiC matrix (2D SiC/SiC) composite was prepared by polymer infiltration-pyrolysis (PIP). Matrix cracking mechanisms of the composite were investigated by in situ SEM and nano-CT to grasp tensile damage evolution. Results showed that PIP-SiC matrix possessed low-fracture energy with non-homogeneous distribution, leading to simultaneous initiation of matrix cracking outside transverse fiber bundles and in unreinforced regions. Cracks then got deflected along weak fiber/matrix interface, which accelerated crack proliferation within the composite. With an increase in the stress, cracks subsequently deflected along plain-woven layers and converged to form longitudinal macrocracks. The composite was finally delaminated via sliding.     

Abnormal mechanical hysteresis behavior of Tyranno-ZMI SiC/SiC containing Ti3Si(Al)C2

This work studied the effect of tough phase Ti₃Si(Al)C₂ on the mechanical hysteresis behavior of SiC/SiC. Different from continuous fibers reinforced brittle ceramic matrix composites, the mechanical hysteresis behavior of SiC/SiC containing Ti₃Si(Al)C₂ shows some abnormal phenomena: as peak applied stress increases during cyclic loading-unloading-reloading tests, the thermal residual stress values exhibit highly dispersion and the thermal misfit relief strain shows abnormally slow growth. These abnormal phenomena are caused by the reduction of transvers cracks (perpendicular to loading fibers) and the generation of hoop cracks (parallel to loading fibers). The plastic deformations of Ti₃Si(Al)C₂ prevents the transverse cracking of modified matrix, while promoting the hoop cracking of SiC matrix prepared by chemical vapor infiltration (CVI-SiC). Hoop cracking occurs within the transition zone containing amorphous SiO₂ layer and carbon layer in CVI-SiC matrix. The combination of weak transition zone and strong modified matrix finally leads to the occurrence of hoop cracking.     

Preparation of SiC/SiC composites with high toughness by reaction of the SiCP+C double-cladding layer with liquid silicon

SiC/SiC composites prepared by liquid silicon infiltration (LSI) have the advantages of high densification, matrix cracking stress and ultimate tensile strength, but the toughness is usually insufficient. Relieving the residual microstress in fiber and interphase, dissipating crack propagation energy, and improving the crystallization degree of interphase can effectively increase the toughness of the composites. In this work, a special SiC particles and C (SiC_P +C) double-cladding layer is designed and prepared via the infiltration of SiC_P slurry and chemical vapor infiltration (CVI) of C in the porous SiC/SiC composites prepared by CVI. After LSI, the SiC generated by the reaction of C with molten Si combines with the SiC_P to form a layered structure matrix, which can effectually relieve residual microstress in fiber and interphase and dissipate crack propagation energy. The crystallization degree of BN interphase is increased under the effects of C-Si reaction exotherm. The as-received SiC/SiC composites possess a density of 2.64 g/cm³ and a porosity of 6.1%. The flexural strength of the SiC/SiC composites with layered structure matrix and highly crystalline BN interphase is 577 MPa, and the fracture toughness reaches up to 37 MPa·m^1/2. The microstructure and properties of four groups of SiC/SiC composites prepared by different processes are also investigated and compared to demonstrate the effectiveness of the SiC_P +C double-cladding layer design, which offers a strategy for developing the SiC/SiC composites with high performance.     

Electrical Resistance of SiC Fiber Reinforced SiC/Si Matrix Composites at Room Temperature during Tensile Testing

The implementation of Ceramic Matrix Composites necessitates the understanding of stress‐dependent damage evolution. Toward this goal, two liquid silicon infiltrated SiCf reinforced SiC composites were tensile tested with electrical resistance (ER) monitoring as well as acoustic emission to quantify matrix cracking. ER was modeled using a combination of resistors in series and parallel to model transverse matrix cracks and fiber/matrix segments between matrix cracks. It is shown that resistance change is sensitive to transverse matrix crack formation and stress‐dependent debonding length. The model appears to be accurate up to the stress for matrix crack saturation.     

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.     

Compressive strength and damage mechanisms of 2D-C/SiC composites at high temperatures

Compressive strength of 2D-C/SiC composite was investigated from room temperature(RT) to 1600?°C at present work. Damage evolution was investigated by conducting loading/unloading tests at RT and the damage mechanisms were elucidated by observing the fracture morphology. It is found that compressive strength of 2D-C/SiC was retained until 1200?°C and then decreased with increasing temperature. The variation of compressive strength is closely related to the degradation in matrix modulus. The compressive damage of 2D-C/SiC starts at the buckling of 0° fiber and is followed by opening and closing of original pores, initiation and growth of longitudinal interbundle cracks, separation of 90° fiber bundles by longitudinal cracks, matrix cracking from intrabundle pores, propagation of matrix cracks into 0° fiber bundles, connection of cracks in 0° fiber bundles and longitudinal cracks in 90° fiber bundles.     

Interpreting acoustic energy emission in SiC/SiC minicomposites through modeling of fracture surface areas

The relationship between acoustic emission (AE) and damage source areas in SiC/SiC minicomposites was modeled using insights from tensile testing in-scanning electron microscope (SEM). Damage up to matrix crack saturation was bounded by: (1) AE generated by matrix cracking (lower bound) and (2) AE generated by matrix cracking, and fiber debonding and sliding in crack wakes (upper bound). While fiber debonding and sliding exhibit lower strain energy release rates than matrix cracking and fiber breakage, they contribute significant damage area and likely produce AE. Fiber breaks beyond matrix crack saturation were modeled by two conditions: (i) only fiber breaks generated AE; and (ii) fiber breaks occurred simultaneously with fiber sliding to generate AE. While fiber breaks are considered the dominant late-stage mechanism, our modeling indicates that other mechanisms are active, a finding that is supported by experimental in-SEM observations of matrix cracking in conjunction with fiber failure at rupture.     

Study on interfacial debonding stress and damage mechanisms of C/SiC composites using acoustic emission

Among ceramic matrix composites (CMCs), carbon fiber-reinforced silicon carbide matrix (C/SiC) composites are widely used in numerous high-temperature structural applications because of their superior properties. The fiber–matrix (FM) interface is a decisive constituent to ensure material integrity and efficient crack deflection. Therefore, there is a critical need to study the mechanical properties of the FM interface in applications of C/SiC composites. In this study, tensile tests were conducted to evaluate the interfacial debonding stress on unidirectional C/SiC composites with fibers oriented perpendicularly to the loading direction in order to perfectly open the interfaces. The characteristics of the material damage behaviors in the tensile tests were successfully detected and distinguished using the acoustic emission (AE) technique. The relationships between the damage behaviors and features of AE signals were investigated. The results showed that there were obviously three damage stages, including the initiation and growth of cracks, FM interfacial debonding, and large-scale development and bridging of cracks, which finally resulted in material failure in the transverse tensile tests of unidirectional C/SiC composites. The frequency components distributed around 92.5 kHz were dominated by matrix damage and failure, and the high-frequency components distributed around 175.5 kHz were dominated by FM interfacial debonding. Based on the stress and strain versus time curves, the average interfacial debonding stress of the unidirectional C/SiC composites was approximately 1.91 MPa. Furthermore, scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDXS) were used to observe the morphologies and analyze the chemical compositions of the fractured surfaces. The results confirmed that the fiber was completely debonded from a matrix on the fractured surface. The damage behaviors of the C/SiC composites were mainly the syntheses of matrix cracking, fiber breakage, and FM interfacial debonding.     

A chemo-mechanical coupled constitutive model applied to the oxidation simulation of SiC/SiC composite

Herein, a chemo-mechanical coupled constitutive and failure model is proposed to predict the tensile behavior of SiC/SiC composites under oxidizing environments. The diffusion of O₂ through the oxide scale and the oxidation reaction of SiC/O₂ are modeled and implemented in finite element software, through a user-defined element. Numerical validation studies and tests are conducted on a domestic SiC fiber. An orthotropic constitutive model for reinforcements, which considers modulus reduction due to oxidation damage, and a continuum damage model associated with O₂ diffusion along the micro-cracks in the SiC matrix are subsequently presented. The developed framework is used to simulate the mechanical behavior and oxidation process of a single fiber SiC/SiC composite.     

裂解碳包覆对SiC纳米纤维增强SiC陶瓷基复合材料性能的影响

以SiC纳米纤维(SiC_nf)为增强体,通过化学气相沉积在SiC纳米纤维表面沉积裂解碳(PyC)包覆层,并与SiC粉体、Al₂O₃-Y₂O₃烧结助剂共混制备陶瓷素坯,采用热压烧结工艺制备质量分数为10%的SiC纳米纤维增强SiC陶瓷基(SiC_nf/SiC)复合材料。研究了PyC包覆层沉积时间对SiC_nf/SiC陶瓷基复合材料的致密度、断裂面微观形貌和力学性能的影响。结果表明:在1 100 ℃下沉积60 min制备的PyC包覆层厚度为10 nm,且为结晶度较好的层状石墨结构;相比于纤维表面无包覆层的复合材料,复合材料的断裂韧性提高了35%,达到最大值(19.35±1.17) MPa·m^1/2,抗弯强度为(375.5±8.5) MPa,致密度为96.68%。复合材料的断裂截面可见部分纳米纤维拔出现象,但SiC_nf/SiC陶瓷基复合材料界面结合仍较强,纳米纤维拔出短,表现为脆性断裂。     

Matrix cracking onset stress and strain as a function of temperature,and characterisation of damage modes in SiCf/SiC ceramic matrix composites via acoustic emission

The complex damage mechanisms that accumulate within SiC_f/SiC ceramic matrix composites (CMCs) subject to thermal and mechanical stress are being investigated in anticipation of the material’s introduction into high performance gas turbine engines. Acoustic emission (AE) is recognised as a leading non-destructive evaluation (NDE) tool to this end, and was used in this study to determine the so-called matrix cracking onset stress under tensile load as a function of temperature up to a maximum of 1100 °C. Onset stress was interpreted using three traditional measurements based on AE energy characteristics during monotonic tests to failure. Pattern recognition (PR) analysis was performed on the AE data, revealing a specific cluster of signals that correlated closely with the initial matrix cracking region of the stress-strain curve. Taken in isolation, the onset stress of this activity was significantly lower than the conventional value. PR results were investigated further, and isolated clusters were linked to damage modes anticipated at other specific regions of the stress history. A secondary series of experiments was performed on specimens representing the individual constituents of the CMC (single-phase SiC flexural bars, Hi-Nicalon? fibre bundles and SiC_f/SiC mini-composites) in attempts to further validate the corresponding AE signal characteristics. Matrix cracking and interphase debonding/sliding damage modes could be identified consistently, while fibre breaks remained difficult to isolate under the current experimental conditions.     

Removal mechanism of SiC/SiC composites by underwater femtosecond laser ablation

Silicon carbide Ceramic matrix composites (SiC matrix with SiC fibers, abbreviated as SiC/SiC composites) are widely used in aerospace and energy applications due to their excellent resistance to high temperatures, corrosion, wear, and low density. However, the difficult machinability and surface oxidation of SiC/SiC composites are the main factors restricting their further application. To address these issues, this paper explores a novel method for underwater femtosecond laser ablation of SiC/SiC composites to obtain high cleanliness, low-oxidation microporous surfaces. This paper systematically analyses the changes in hole depth, material removal rate (MRR), surface morphology, and material components during underwater femtosecond laser ablation of SiC/SiC composites, and explains the formation of typical features such as induced cones, small banded pits, fiber debonding and shedding. Our work provides new research ideas for understanding the removal mechanism and surface oxidation resistance of SiC/SiC composites.     

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.     

Study of material removal mechanisms in grinding of C/SiC composites via single-abrasive scratch tests

As one of the ceramic matrix composites (CMCs), carbon fiber-reinforced silicon carbide matrix (C/SiC) composites are promising materials used in various engineering applications owing to their superior properties. Precision surface grinding has been widely applied in the machining of CMC composites; however, the material removal mechanisms of C/SiC composites have not been fully elucidated yet. To reveal the material removal mechanisms in the grinding of chemical vapor infiltration-fabricated C/SiC composites, novel single-abrasive scratch tests were designed and conducted in two typical cutting directions. The experimental parameters, especially the cutting speed, conformed to the actual grinding process. The results show that the grinding parameters (feed rate, spindle speed, depth of cut, and cutting direction) have significant influences on the grinding forces, surface integrity, and affected subsurface region. The tangential force is in general larger than the normal force at the same cutting depth. Furthermore, both the tangential and normal forces in the longitudinal cutting direction are larger than those in the transverse cutting direction. The impacts and abrasive actions at the tool tip mainly caused the material removal. The predominant material removal mode is brittle fracture in the grinding of unidirectional C/SiC composites, because the damage behaviors of the C/SiC composites are mainly the syntheses of matrix cracking, fiber breakage, and fiber/matrix interfacial debonding. These results are rationalized based on the composite properties and microstructural damage features.     

Ni包裹SiC对SiC(Ni)/Fe复合材料性能的影响

分别以SiC粉体和Ni包裹的SiC复合粉体为硬质相,采用热压工艺(1000°C,20°C/min,40 MPa和45 min)制备了SiC含量为1 wt%~9 wt%的SiC/Fe复合材料。采用扫描电镜(SEM)、能谱仪(EDS)和X射线衍射仪(XRD)等研究了复合材料的界面反应物。研究结果表明:Ni过渡层的存在有效避免了SiC颗粒与Fe基体之间的化学反应。随着Ni包裹SiC粉体含量的增加,复合材料的相对密度和抗弯强度先增加后减小,当SiC(Ni)粉体含量为5 wt%时达到最大值。     

基于深度学习的平纹Cf/SiC复合材料原位拉伸损伤演化与断裂分析

为揭示平纹C_f/SiC复合材料的拉伸损伤演化及失效机理,开展了X射线CT原位拉伸试验,获得材料的三维重构图像,利用深度学习的图像分割方法,准确识别出拉伸裂纹并实现其三维可视化。分析了平纹C_f/SiC复合材料损伤演化与失效机理,基于裂纹的三维可视化结果对材料损伤进行了定量表征。结果表明:平纹C_f/SiC复合材料的拉伸力学行为呈现非线性,拉伸过程中主要出现基体开裂、界面脱黏、纤维断裂及纤维拔出等损伤;初始缺陷易引起材料损伤,孔隙多的部位裂纹数量也多;纤维束外基体裂纹可扩展至纤维束内部,并发生裂纹偏转。基于深度学习的智能图像分割方法为定量评估陶瓷基复合材料损伤演化与失效机理提供了有效分析手段。     

SiC基高性能材料的研究进展

作为先进高温结构陶瓷材料的典型代表SiC烧结体材料具有优良的性能,应用十分广泛,但是,单一的SiC烧结体材料的断裂韧性低和难以烧结致密的缺点使得其应用受到一定的限制。近年来,研究SiC材料在结构材料方面的应用大多倾向于SiC基复合材料方向发展。本文介绍了纤维补强型和颗粒弥散增强型SiC基复合材料近五六年来的研究情况。     

Strengthening/toughening of 2D C/SiC composites by coating

SiC and SiC_w/SiC coatings were prepared on two-dimensional carbon fiber reinforced silicon carbide ceramic matrix composites (2D C/SiC), and strengthening/toughening of the composite by the coatings was investigated. After coating, the density of the C/SiC composites was increased effectively and the mechanical properties were improved significantly. Compared with SiC coating, SiC_w/SiC coating showed the more significant effect on strength/toughness of the composites. Coatings had two effects: surface strengthening and matrix strengthening. The latter was the dominant effect. The surface strengthening can increase the crack initiation stress, while the matrix strengthening can enhance the crack propagation resistance. The former effect increased the strength and the latter effect increased the toughness.     

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.