Hysteresis loops of carbon fiber-reinforced ceramic-matrix composites with different fiber preforms

The hysteresis loops of C/SiC ceramic-matrix composites (CMCs) with different fiber preforms, i.e., unidirectional, cross-ply, 2D and 2.5D woven, 3D braided, and 3D needled at room temperature have been investigated. Based on fiber slipping mechanisms, the hysteresis loops models considering different interface slip cases have been developed. The effects of fiber volume fraction, matrix cracking density, interface shear stress, interface debonded energy, and fibers failure on hysteresis loops, hysteresis dissipated energy, hysteresis width, and hysteresis modulus have been analyzed. An effective coefficient of fiber volume fraction along the loading direction (ECFL) was introduced to describe fiber preforms. The hysteresis loops, hysteresis dissipated energy and hysteresis modulus of unidirectional, cross-ply, 2D and 2.5D woven, 3D braided and 3D needled C/SiC composites have been predicted.     

High temperature bending properties and failure mechanism of 3D needled C/SiC composites up to 2000 ℃

Three-dimensional (3D) needled C/SiC composites were prepared and subjected to three-point bending tests from room temperature (RT) to 2000 ℃ under vacuum. The results show that the flexural strength and modulus increase in the range of RT to 800 °C due to the release of thermal residual stress (TRS). At 800–1700 °C, the modulus further increases for the further release of TRS, while the destruction of the pyrolytic carbon (PyC) coating reduces the flexural strength. Up to 2000 ℃, the thermal mismatch stress in the composites cause fiber slippage and matrix crack deflection to be zigzag, which increase the fracture strength. The change of components properties mediated by high temperature and the release of TRS play a leading role in the flexural strength and fracture mode. The results provide important support for the mechanical behavior of 3D needled C/SiC composites at ultra-high temperature.     

Fabrication and characterization of carbon fiber reinforced SiC ceramic matrix composites based on 3D printing technology

A novel method has been developed to fabricate carbon fiber reinforced SiC (C_f/SiC) composites by combining 3D printing and liquid silicon infiltration process. Green parts are firstly fabricated through 3D printing from a starting phenolic resin coated carbon fiber composite powder; then the green parts are subjected to vacuum resin infiltration and pyrolysis successively to generate carbon fiber/carbon (C_f/C) preforms; finally, the C_f/C preforms are infiltrated with liquid silicon to obtain C_f/SiC composites. The 3D printing processing parameters show significant effects on the physical properties of the green parts and also the resultant C_f/C preforms, consequently greatly affecting the microstructures and mechanical performances of the final C_f/SiC composites. The overall linear shrinkage of the C_f/SiC composites is less than 3%, and the maximum density, flexural strength and fracture toughness are 2.83?±?0.03?g/cm³, 249?±?17.0?MPa and 3.48?±?0.24?MPa m^1/2, respectively. It demonstrates the capability of making near net-shape C_f/SiC composite parts with complex structures.     

The effects of preparation temperature on the SiCf/SiC 3D4d woven composite

Continuous silicon carbide fiber reinforced silicon carbide matrix (SiC_f/SiC) composites have promising applications in aero-engine due to their unique advantages, such as low density, high modulus and strength, outstanding high temperature resistance and oxidation resistance. As SiC fibers are main reinforcements in SiC_f/SiC composites, the crystallization rate and initial damage degree of SiC fibers are seriously influenced by preparation temperatures of SiC_f/SiC composites, namely mechanical properties of SiC fibers and SiC_f/SiC composites are influenced by preparation temperatures. In this paper, KD-II SiC fibers were woven into 3D4d preforms and SiC matrix was fabricated by PIP process at 1100 °C, 1200 °C, 1400 °C and 1600 °C. Digital image correlation (DIC) method was adopted to measure the uniaxial tensile properties of these SiC_f/SiC composites. In addition, finite element method (FEM) based on representative volume element (RVE) was adopted to predict the mechanical properties of SiC_f/SiC composites. The good agreements between numerical results and experimental results of uniaxial tensile tests verified the validity of the RVE. In last, the transverse tensile, transverse shear, uniaxial shear properties were predicted by this method. The predicted results illustrated that axial tensile, transverse tensile and axial shear properties were greatly influenced by the preparation temperatures of SiC_f/SiC composites while transverse shear properties were not significantly various. And the mechanical properties of SiC_f/SiC composites peaked at 1200 °C among these four temperatures while their values reached their lowest points at 1600 °C because of thermal damage and brittle failure of SiC_f/SiC composites.     

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.     

Microstructural evolution and mechanical performances of SiC/SiC composites by polymer impregnation/microwave pyrolysis (PIMP) process

SiC/SiC composites were prepared by polymer impregnation/microwave pyrolysis (PIMP) process, and their microstructural evolution and the mechanical performances were characterized. Using non-coated Tyranno SA fiber preforms as reinforcement and impregnation with only allylperhydropolycarbosilane (AHPCS) into the preforms, Tyranno SA/SiC composite (TSA/SiC) with higher density was obtained. While using carbon-coated Tyranno SA fiber preforms, Tyranno SA/C/SiC composite (TSA/C/SiC) with lower density were also fabricated. In this composite, SiC particulate was loaded with polymer precursor (AHPCS) in the first cycle impregnation. Microstructural observation revealed that pore and crack formation was affected by processing conditions. Bending strength was also dependent on the microstructural evolution of the samples. In TSA/SiC composite, relatively strong interfaces contribute to effective load transfer so that higher bending strength could be reached. In the TSA/C/SiC composite, weak interfaces provide a relatively lower strength. Meanwhile, different microstructural evolution and interfacial properties of the composites lead to the variation of the fracture behaviors.     

化学气相渗透法制备2维和2.5维C/SiC复合材料及其拉伸性能

采用化学气相渗透法制备了2维和2.5维碳纤维增强碳化硅(carbon-fiber-reinforced silicon carbide,C/SiC)复合材料,沿经纱(纵向)和纬纱(横向) 2个方向对2种复合材料进行了室温拉伸性能测试,并从预制体结构和原始缺陷分布的角度对比分析了两者力学性能之间的差异.结果表明:两种C/SiC复合材料均表现出明显的非线性力学行为,在经纱方向和纬纱方向上,2维C/SiC复合材料力学性能表现为各向同性,而2.5维C/SiC复合材料力学性能则表现出明显的各向异性:经纱方向上2.5维C/SiC复合材料的拉伸强度和拉伸模量(326 MPa,153 GPa)均高于2维C/SiC复合材料的(245 MPa,96 GPa),纬纱方向上的(145 MPa,62 GPa)均低于2维C/SiC复合材料的(239 MPa,90 GPa).两种复合材料的拉伸断裂行为均表现为典型的韧性断裂,并伴有大量的纤维拔出.两种复合材料中纱线断裂均呈现出多级台阶式断裂方式,但其断裂位置并不相同.2.5维C/SiC复合材料中由于经纱路径近似于正弦波,弯曲程度较大,在纱线交叉点处造成明显的应力集中,因此经纱多在纱线交叉点处断裂;而纬纱由于其路径近乎直线,应力集中现象不明显,因此纬纱断裂位置呈随机分布.2维C/SiC复合材料中经纱和纬纱由于其路径类似于2.5维C/SiC复合材料中的经纱,因此其断裂位置也多在纱线交叉点处.微观结构观察表明不同的编织结构是造成两种复合材料在不同方向上力学性能差异的主要原因.     

Effects of density and heat treatment of C/C preforms on microstructure and mechanical properties of C/C–SiC composites

Twill multidirectional carbon-fiber-reinforced carbon and silicon carbide composites (i.e., C/C–SiC) were prepared via chemical vapor infiltration combined with reactive melt infiltration process. The effect of heat treatment (HT) on the microstructure and mechanical properties of C/C–SiC composites obtained by C/C preforms with different densities was thoroughly investigated. The results show that as the bulk density of C/C preforms increases, the thickness of the pyrolytic carbon (PyC) layer increases and open pore size distribution narrows, making the bulk density and residual silicon content of C/C–SiC composites decrease. Moreover, the flexural strength and tensile strength of the C/C–SiC composites were improved, which can be attributed to the increased thickness of the PyC layer. The compressive strength reduces due to the decrease of the ceramic phase content. HT improves the graphitization degree of PyC, which reduces the silicon–carbon reaction rate and thereby the content of the SiC phase. HT induces microcracks and porosity but not obviously affects the mechanical properties of C/C–SiC composites. However, the negative impact of HT can be compensated by the increased density of the C/C preforms.     

Creep properties of melt infiltrated SiC/SiC composites with Sylramic™-iBN and Hi-Nicalon™-S fibers

Isothermal tensile creep tests were conducted on 2D woven and laminated, 0/90 balanced melt infiltration (MI) SiC/SiC composites at stress levels from 48 to 138 MPa and temperatures to 1400°C in air. Effects of fiber architecture and fiber types on creep properties, influence of accumulated creep strain on in-plane tensile properties, and the dominant constituent controlling the creep behavior and creep rupture properties of these composites were investigated. In addition, the creep parameters of both composites were determined. Results indicate that in 2D woven MI SiC/SiC composites with Sylramic™-iBN or Hi-Nicalon™-S fibers, creep is controlled by chemical vapor infiltration (CVI) SiC matrix, whereas in 2D laminated MI SiC/SiC composites with Hi-Nicalon™-S fibers, creep is controlled by the fiber. Both types of composites exhibit significant variation in creep behavior and rupture life at a constant temperature and stress, predominantly due to local variation in microstructural inhomogeneity and stress raisers. In both types of composites at temperatures >1350°C, residual silicon present in SiC matrix to reacts with SiC fibers and fiber coating causing premature creep rupture. Using the creep parameters generated, the creep behaviors of the composites have been modeled and factors influencing creep durability are discussed.     

Wet oxidation behavior of SiC/(SiC- SiBCN)x composites prepared by CVI combined with PIOP process

Self-healing capability in wet oxygen atmospheres is the key issue for long term service of SiC/SiC composites in aero-engines. Polymer derived SiBCN ceramic (PDC SiBCN) was introduced into SiC fiber reinforced SiC as a self-healing component to obtain SiC/(SiC-SiBCN)x composites by a newly developed method, namely chemical vapor infiltration combined with polymer infiltration online pyrolysis (CVI + PIOP) process. The weight loss behavior and three-point bending performance of the samples under different temperatures (1200, 1300 and 1400°C) and different wet oxygen partial pressures were tested up to 100 hours to demonstrate the oxidation behavior of the samples in wet oxygen environments. According to these tests, the antioxidant capacities of samples prepared from different preforms were compared. It has been found that the 2D plain weave samples with higher density have the best resistance to wet oxygen corrosion while the 2D plain weave samples have the worst resistance to wet oxidation and the antioxidant capacities of 2D satin weave samples is between them.     

In-plane thermal expansion behavior of dense ceramic matrix composites containing SiBC matrix

In order to reveal the effect of matrix cracks resulted from thermal residual stresses (TRS) on the thermal expansion behavior of ceramic matrix composites, SiBC matrix was introduced into C_f/SiC and SiC_f/SiC by liquid silicon infiltration. The TRS in both two composites were enlarged with incorporating SiBC matrix which has higher coefficients of thermal expansion (CTEs) than SiC matrix. Due to the relatively high TRS, matrix cracks and fiber/matrix (f/m) debonding exist in C_f/SiC-SiBC, which would provide the space for the expansion of matrix with higher CTEs. For SiC_f/SiC, no matrix cracking and f/m debonding took place due to the close CTEs between fiber and matrix. Accordingly, with the incorporation of SiBC matrix, the in-plane CTE of C_f/SiC between room temperature to 1100 °C decreases from 3.65 × 10⁻⁶ to 3.19 × 10⁻⁶ K^-1, while the in-plane CTE of SiC_f/SiC between room temperature to 1100 °C increases slightly from 4.97 × 10⁻⁶ to 5.03 × 10⁻⁶ K^-1.     

A multiscale modeling for predicting the thermal expansion behaviors of 3D C/SiC composites considering porosity and fiber volume fraction

Coefficients of thermal expansion (CTEs) are an essential design criterion of the three-dimensional carbon fiber reinforced SiC matrix composites (3D C/SiC). Representative volume element (RVE) models of microscale, void/matrix, and mesoscale developed in this work were used to investigate the CTEs of these composites. A coupled temp-displacement steady-state analysis step was created for assessing the thermal expansions behaviors of the composites by applying periodic displacement and temperature boundary conditions. Three RVE models of cuboid, hexagonal and fiber random distribution were respectively established to comparatively study the influence of fiber package pattern on the CTEs at microscale. Similarly, the effects of different void size, locations, and shapes on the CTEs of the matrix are comparatively analyzed by the void/matrix models. The prediction results at mesoscale corresponded closely to the experimental results. The effect of the porosities on the CTEs was studied by the void/matrix RVE models. The voids were effective in lowering the CTE of the 3D C/SiC composites. Furthermore, the effect of fiber volume fractions on the CTE were also taken into consideration. Equal in-plane and out-of-plane CTEs were realized by selecting appropriate fiber volume fractions for the different directions. The multiscale models developed in this work can be used to predict the thermal expansion behaviors of other complex structure composites.     

三维针刺C/SiC复合材料无纬布纤维方向对材料力学性能的影响

通过化学气相渗透法结合反应熔体浸渗法制备了三维针刺C/SiC复合材料,采用扫描电子显微镜观察材料的显微结构,并研究了无纬布纤维方向对材料力学性能的影响.结果表明,三维针刺C/SiC复合材料由O°无纬布层、短纤维胎网层、90°无纬布层以及针刺纤维束组成,无纬布层纤维方向对材料性能有显著影响.试样的拉伸强度和弯曲强度随着无纬布纤维方向与试样长度方向的夹角θ(0 ～45°)值的增大而减小,面内剪切强度和冲击韧性随θ角的增大而增大.     

Microstructure observation and analysis of 3D carbon fiber reinforced SiC-based composites fabricated through filler enhanced polymer infiltration and pyrolysis

3D C/SiC-BN composites were fabricated by filler enhanced polymer infiltration and pyrolysis (FE-PIP) through in situ conversion of active filler boron into h-BN in the high temperature treatment process. The bending strengths and microstructures of composites were studied here. Interphase layers deposited on the fiber surfaces can prevent the strong bonding between fiber reinforcements and composite matrix and repair the defects on the fiber surface, which can improve the bending strength and toughness of composites. The bending stress of C/SiC-BN composites without interphase layer is about 170 MPa while those of composites with PyC or PyC/SiC interphase layers are higher than 300 MPa. Some large pores were left in the interwoven zones while intra-bundle zones were relatively dense, only a small amount of micro-pores could be observed. It could also be concluded that the length of pulled-out fibers was much longer and the pulled-out fiber surface was smoother when interphase layers were deposited. Because the matrix derived from the pyrolysis of slurries adheres to the fiber bundles, some phases with layered structures could be observed in the matrix near the reinforcements. The microstructure evolution of 3D fiber reinforced ceramic matrix composites were also analyzed in this work based on the observation of both 3D C/SiC-BN composites and 3D C/SiC composites fabricated by FE-PIP, where boron and SiC particles were applied as active fillers and inert fillers respectively.     

Fabrication and properties of Cf/ZrC‐SiC‐based composites by an improved reactive melt infiltration

C_f/ZrC‐SiC composites with a density of 2.52 g/cm³ and a porosity of 1.68% were fabricated via reactive melt infiltration (RMI) of Si into nano‐porous C_f/ZrC‐C preforms. The nano‐porous C_f/ZrC‐C preforms were prepared through a colloid process, with a ZrC “protective coating” formed surrounding the carbon fibers. Consequently, highly dense C_f/ZrC‐SiC composites without evident fiber/interphase degradation were obtained. Moreover, abundant needle‐shaped ZrSi₂ grains were formed in the composites. Benefiting from this unique microstructure, flexural strength, and elastic modulus of the composites are as high as 380 MPa and 61 GPa, respectively, which are much higher than C_f/ZrC‐SiC composites prepared by conventional RMI.     

Modeling matrix multicracking development of fiber-reinforced ceramic-matrix composites considering fiber debonding

In this paper, the effect of fiber debonding on matrix multicracking development of different fiber-reinforced CMCs is investigated using the micromechanical approach. The Budiansky–Hutchinson–Evans shear-lag model is adopted to analyze the fiber and matrix stress distributions of the damaged composite. The fracture mechanics approach is used to determine the fiber/matrix interface debonding length. Combining the critical matrix strain energy criterion and fracture mechanics fiber/matrix interface debonding criterion, the stress-dependent matrix multicracking development is analyzed for different fiber volume fraction, fiber/matrix interface properties and matrix cracking characteristic stress. The experimental matrix multicracking development of unidirectional C/Si₃N₄, SiC/Si₃N₄, SiC/CAS, SiC/CAS-II, SiC/SiC, SiC/Borosilicate and mini-SiC/SiC composites are predicted.     

Effect of multiple loading sequence on time-dependent stress rupture of fiber-reinforced ceramic-matrix composites

In this paper, the effect of multiple loading sequence on time-dependent stress rupture of fiber-reinforced ceramic-matrix composites (CMCs) at intermediate temperatures in oxidative environment is investigated. Considering multiple damage mechanisms, a micromechanical constitutive model for time-dependent stress rupture is developed to determine damage evolution of matrix crack spacing, interface debonding and oxidation length, and fiber failure probability under single and multiple loading sequences. The relationships between multiple loading sequence, composite strain evolution, time, matrix cracking, interface debonding and oxidation, and fiber fracture are established. The effects of fiber volume, matrix crack spacing, interface shear stress in the slip and oxidation region, and environment temperature on the stress/time-dependent strain, interface debonding and oxidation fraction, and fiber broken fraction of SiC/SiC composite are analyzed. The experimental stress rupture of SiC/SiC composite under single and multiple loading sequences at 950°C in air atmosphere is predicted. Compared with single loading stress, multiple loading sequence affects the interface debonding and oxidation fraction in the debonding region, leading to the higher fiber broken fraction and shorter stress-rupture lifetime.     

Three-Dimensional Carbon/Silicon Carbide Composites Prepared by Chemical Vapor Infiltration

Continuous-carbon-fiber-reinforced silicon carbide composites (C/SiC) were prepared by chemical vapor infiltration in which the preforms were fabricated with the three-dimensional braid method. The mechanical properties and microstructures were investigated. For the composites with no interfacial layer, flexural strength and fracture toughness increased with density of the composites, and the maximum values were 520 MPa and 16.5 MPa·m^1/2, respectively. The fracture behavior was dependent on the interfacial bonding between fiber/matrix and fiber bundle/bundle which was determined by the density of the composites. Heat treatment had a significant influence on the mechanical properties and fracture behavior. The composites with pyrolysis interfacial layers exhibited characteristic fracture and relatively low strength (300 MPa).     

Ring compression properties of SiCf/SiC composites prepared by chemical vapor infiltration

SiC fiber reinforced SiC matrix (SiC_f/SiC) composites prepared by chemical vapor infiltration are one of promising materials for nuclear fuel cladding tube due to pronounced low radioactivity and excellent corrosion resistance. As a structure component, mechanical properties of the composites tubes are extremely important. In this study, three kinds of SiC_f preform with 2D fiber wound structure, 2D plain weave structure and 2.5D shallow bend-joint structure were deposited with PyC interlayer of about 150–200?nm, and then densified with SiC matrix by chemical vapor infiltration at 1050?°C or 1100?°C. The influence of preform structure and deposition temperature of SiC matrix on microstructure and ring compression properties of SiC_f/SiC composites tubes were evaluated, and the results showed that these factors have a significant influence on ring compression strength. The compressive strength of SiC_f/SiC composites with 2D plain weave structure and 2.5D shallow bend-joint structure are 377.75?MPa and 482.96?MPa respectively, which are significantly higher than that of the composites with 2D fiber wound structure (92.84?MPa). SiC_f/SiC composites deposited at 1100?°C looks like a more porous structure with SiC whiskers appeared when compared with the composites deposited at 1050?°C. Correspondingly, the ring compression strength of the composites deposited at 1100?°C (566.44?MPa) is higher than that of the composites deposited at 1050?°C (482.96?MPa), with a better fracture behavior. Finally, the fracture mechanism of SiC_f/SiC composites with O-ring shape was discussed in detail.     

Modelling shear behaviors of 2D C/SiC z-pinned joint prepared by chemical vapor infiltration

Progressive failure model is developed to investigate shear behaviors of 2D C/SiC z-pinned joint prepared by chemical vapor infiltration (CVI). It includes progressive failure model of 2D C/SiC composites and cohesive model of faying plane, in order to describe joint nonlinear shear behaviors and z-pin shear-off failure mode, respectively. All cohesive parameters are directly obtained from mechanical properties of 2D C/SiC composites. Results show that the model can almost reproduce joint shear behaviors and z-pin shear-off failure process. Joint failure results from coupled fiber tensile and fiber–matrix shearing damages at faying plane. The model also successfully demonstrates that joint shear properties can be effectively improved by changing z-pin density and diameter. The relationship between joint properties and mechanical properties of 2D C/SiC composites are subsequently obtained with the model. In this sense, joint shear strength increases with cohesive or in-plane shear strengths of 2D C/SiC composites.