不同界面SiC/SiC复合材料的断裂行为研究

碳化硅纤维增强碳化硅复合材料(SiC/SiC)是极具前景的高温结构材料。通过先驱体浸渍裂解(PIP)工艺分别制备了PyC界面和CNTs界面SiC/SiC复合材料, 对两种SiC/SiC复合材料的整体力学性能以及界面剪切强度等进行了测试表征, 并对材料中裂纹的产生与扩展进行了原位观测。结果表明, 两种界面SiC/SiC复合材料弯曲强度相近, 但PyC界面SiC/SiC复合材料的断裂韧性约为CNTs界面SiC/SiC复合材料的两倍。在PyC界面SiC/SiC复合材料中, 裂纹沿纤维-基体界面扩展, PyC涂层能够偏转或阻止裂纹, 材料呈现伪塑性断裂特征; 而在CNTs界面SiC/SiC复合材料中, 裂纹在扩展路径上遇到界面并不偏转, 初始裂纹最终发展为主裂纹, 材料呈现脆性断裂模式。     

PyC/SiC界面相对PIP法制备3D HTA C/SiC复合材料性能的影响

利用三维编织炭纤维预制件通过先驱体浸渍裂解法制备C／SiC复合材料。研究了热解碳（PyC）／SiC界面相对复合材料的微观结构和力学性能的影响。弯曲性能通过三点弯曲法测试，复合材料的断口和抛光面通过扫描电镜观察。结果表明：通过等温化学气相沉积法在纤维表面沉积PyC／SiC界面相以后，复合材料的三点抗弯强度从46MPa提高到247MPa。沉积界面的复合材料断口有明显的纤维拔出现象，纤维与基体之间的结合强度适当，起到了增韧作用；而未沉积界面相复合材料的断口光滑、平整，几乎没有纤维拔出，纤维在热解过程中受到严重的化学损伤，性能下降严重，材料表现为典型的脆性断裂。     

反应热压烧结法制备SiC/Ti3SiC2复合材料及其性能

采用反应热压烧结法制备了SiC/Ti3SiC2复合材料,研究了热压温度、SiC含量及粒度对SiC/Ti3SiC2复合材料相组成、力学性能以及应力-应变行为的影响.结果表明:热压温度影响SiC/Ti3SiC2复合材料相组成;随着热压温度的提高,复合材料的弯曲强度和断裂韧性提高;随SiC含量的增加,SiC/Ti3SiC2复...     

2D-C/SiC复合材料面内剪切性能统计及强度B基准值

针对2D-C/SiC复合材料进行大子样面内剪切实验,研究材料面内剪切模量和强度的分布规律及强度B基准值。运用线性回归结合假设检验的方法,确定2D-C/SiC复合材料面内剪切力学性能的分布规律及参数,对比两种不同经验失效概率得到统计结果;通过观察试样最窄净截面微CT照片及断口电镜扫描照片,解释材料面内剪切强度分散性微观机制,基于分布规律,最终计算得到2D-C/SiC复合材料面内剪切强度威布尔B基准值。结果表明:强度和模量均同时服从威布尔、正态和对数正态分布,且理论模型与实验结果吻合良好,两种经验失效概率不影响力学性能分布规律;面内剪切强度分散性与最窄净截面致密度和界面脱粘长度有关;2D-C/SiC复合材料面内剪切强度威布尔B基准值为80.41MPa。     

预制体结构及界面对三维SiC/SiC复合材料拉伸性能的影响

为研究预制体结构及界面对三维编织SiC/SiC复合材料拉伸性能的影响,采用先驱体浸渍裂解法（PIP）分别制备了三维四向和三维五向SiC/SiC复合材料,并引入热解炭/碳化硅（PyC/SiC）复合界面层,进行拉伸性能测试和断口形貌观察。结果表明,三维五向SiC/SiC复合材料拉伸性能优于三维四向SiC/SiC复合材料,三维五向SiC/SiC复合材料的拉伸强度、模量和断裂应变分别是三维四向SiC/SiC复合材料的1.22倍、1.25倍、1.43倍,且比三维四向SiC/SiC复合材料具有更好的强度可靠性。这是由于三维五向SiC/SiC复合材料增加了受力方向的纤维含量,限制了纤维在外力作用下的转动和变形,起到定型和稳固作用。添加PyC/SiC复合界面层,三维五向SiC/SiC复合材料的拉伸强度、模量及断裂应变分别提高了21.7%、15.0%和11.0%。界面的存在可以保护纤维,调节纤维与基体之间的热应力,受力时诱使裂纹偏转和分叉,消耗能量,提高三维五向SiC/SiC复合材料的拉伸性能。      

界面涂层与基体对先进CVI-SiC/SiC复合材料性能的影响

对含有几种典型界面结构和SiC纳米线的CVI-SiC/SiC复合材料的弯曲性能和断裂韧性进行了比较研究. 研究表明: 界面涂层对SiC/SiC的力学性能至关重要, 120nm厚的碳界面涂层使材料的强度与韧性都增加一倍; 在用140nm厚的SiC层将该碳层分为更薄的两层, 形成C/SiC/C多层界面涂层时, 材料的强度没有明显的变化, 而断裂韧性则略有提高. 对基体中弥散分布有SiC纳米线的SiC/SiC的力学性能研究表明, SiC纳米线具有非常高的强化效率, 使SiC/SiC复合材料具有更高的强度和韧性.     

C/SiC复合材料的氧化对其内耗行为的影响

通过分析C/SiC在高温(1250、1300和1350℃)空气氧化过程中质量、强度、物相、气孔率、微观形貌演变规律,并同时采用动态热机械分析仪测得内耗的变化趋势,研究了氧化对其内耗行为的影响规律,进而为以内耗表征复合材料的氧化行为奠定基础.为明确C/SiC各组元在氧化与内耗行为对应关系中所发挥的作用,进一步研究了SiC陶瓷在1300℃、空气中的氧化与内耗行为之间的对应关系.结果表明:SiC陶瓷氧化对其内耗行为的影响规律不明显且影响程度较弱;C/SiC在氧化过程中的内耗行为受C相的氧化损伤控制,且作用规律明显,其内耗保持率曲线均出现峰值,其中1250、1300和1350℃的峰值分别为6.65、3.48和1.59.     

C/SiC复合材料的氧化对其内耗行为的影响

通过分析C/SiC在高温(1250、1300和1350℃)空气氧化过程中质量、强度、物相、气孔率、微观形貌演变规律, 并同时采用动态热机械分析仪测得内耗的变化趋势, 研究了氧化对其内耗行为的影响规律, 进而为以内耗表征复合材料的氧化行为奠定基础。为明确C/SiC各组元在氧化与内耗行为对应关系中所发挥的作用, 进一步研究了SiC陶瓷在1300℃、空气中的氧化与内耗行为之间的对应关系。结果表明: SiC陶瓷氧化对其内耗行为的影响规律不明显且影响程度较弱; C/SiC在氧化过程中的内耗行为受C相的氧化损伤控制, 且作用规律明显, 其内耗保持率曲线均出现峰值, 其中1250、1300和1350 ℃的峰值分别为6.65、3.48和1.59。     

热压烧结制备SiC增强石墨复合材料及其性能

以天然鳞片石墨为起始原料,SiC颗粒为增强相,采用热压烧结工艺制备了SiC增强石墨复合材料。研究了SiC含量对SiC增强石墨复合材料微观结构、力学性能和摩擦性能的影响。结果表明:SiC颗粒均匀分布在石墨基体中,降低了基体中的孔隙率;随着SiC含量增加,SiC增强石墨复合材料的相对密度和弯曲强度相应增加,开孔率显著降低,当SiC含量达到40vol%时,SiC增强石墨复合材料中形成了SiC网络骨架结构,相对密度达到了94.2%,比商品高强纯石墨材料提高了11.8%,弯曲强度达到了146 MPa,比商品高强纯石墨材料提高了147%;基体石墨保持了层状结构;SiC含量低于40vol%时,SiC增强石墨复合材料的摩擦系数随SiC含量的增加轻微增加,与纯石墨材料的摩擦系数相当,具有良好的摩擦性能。     

短切SiC纤维对LAS玻璃陶瓷复合材料性能的影响

采用热压烧结法制备了不同纤维长度的SiCsf/LAS玻璃陶瓷复合材料,研究了该复合材料的微观结构、力学性能和在8.2～12.4GHz频率范围内的微波介电性能.结果表明:SiC纤维体积含量为1%时,随着SiC纤维长度的增加,SiCsf/LAS材料的抗弯强度先增加后降低.由于碳界面层的形成,SiCsf/LAS材料要比LAS材料具有更高的介电常数和损耗.当SiC短纤维的长度为4mm时,SiCsf/LAS复合材料的复介电常数具有最大的频散效应,分析认为这与碳界面层在复合材料中形成的电偶极子有关.     

Mechanical properties of 3D KD-I SiCf/SiC composites with engineered fibre-matrix interfaces

Three-dimensional (3D) silicon carbide (SiC) matrix composites reinforced with KD-I SiC fibres were fabricated by precursor impregnation and pyrolysis (PIP) process. The fibre-matrix interfaces were tailored by pre-coating the as-received KD-I SiC fibres with PyC layers of different thicknesses or a layer of SiC. Interfacial characteristics and their effects on the composite mechanical properties were evaluated. The results indicate that the composite reinforced with as-received fibre possessed an interfacial shear strength of 72.1 MPa while the composite reinforced with SiC layer coated fibres had a much higher interfacial shear strength of 135.2 MPa. However, both composites showed inferior flexural strength and fracture toughness. With optimised PyC coating thickness, the interface coating led to much improved mechanical properties, i.e. a flexural strength of 420.6 MPa was achieved when the interlayer thickness is 0.1 μm, and a fracture toughness of 23.1 MPa m^1/2 was obtained for the interlayer thickness of 0.53 μm. In addition, the composites prepared by the PIP process exhibited superior mechanical properties over the composites prepared by the chemical vapour infiltration and vapour silicon infiltration (CVI-VSI) process.     

Al粉作为活性填料对PIP法SiCf/SiC复合材料性能的影响

利用2.5D SiC纤维预制件,通过前驱体浸渍裂解法（PIP法）制备SiCf/SiC复合材料,通过在第一次浸渍浆料中加入活性Al粉和惰性颗粒SiC粉来提高浸渍效率.研究了活性填料的加入以及纤维表面热解碳层的厚度对材料性能的影响.结果表明,由于Al粉在热解过程中与含碳有机小分子发生化学反应生成新的物相,使得复合材料的力学性能得到了很大的提高,在1200℃经过六个周期的浸渍裂解后,复合材料的三点弯曲强度达到441MPa,比例极限应力达到380MPa.在200～500nm厚度范围内,热解碳的厚度对复合材料的抗弯强度影响不明显.复合材料的弹性模量随着热解碳层厚度的增加而降低.     

Design,Fabrication, Characterization and Simulation of PIP-SiC/SiC Composites

Continuous SiC fiber reinforced SiC matrix composites (SiC/SiC) have been studied and developed for high temperature and fusion applications. Polymer impregnation and pyrolysis (PIP) is a conventional technique for fabricating SiC/SiC composites. In this research, KD-1 SiC fibers were employed as reinforcements, a series of coatings such as pyrocarbon (PyC), SiC and carbon nanotubes (CNTs) were synthesized as interphases, PCS and LPVCS were used as precursors and SiC/SiC composites were prepared via the PIP method. The mechanical properties of the SiC/SiC composites were characterized. Relationship between the interphase shear strength and the fracture toughness of the composites was established. X-ray tomographic scans of the SiC/SiC composites were performed and the closed porosities of the composites were calculated. The compatibility of the SiC/SiC composites with liquid LiPb at 800 °C and 1000 °C was investigated. High-resolution synchrotron X-ray tomography was applied to the SiC/SiC composite and digital volume correlation was employed for Hertzian indentation testing of the SiC/SiC composite. A Cellular Automata integrated with Finite Elements (CAFE) method was developed to account for the effect of microstructure on the fracture behavior of the SiC/SiC composite.     

The effect on the tensile properties of PIP-processed SiC/SiC composite of a chemical vapor-infiltrated SiC layer overlaid on the pyrocarbon interface layer

A chemical vapor-infiltrated (CVI) SiC layer is often deposited on the pyrocarbon (PyC) fiber–matrix interface layer in SiC fiber-reinforced SiC matrix (SiC/SiC) composites. It is normally applied to protect the PyC layer from reacting with molten Si or sintering aids during manufacturing, and to guard against the effects of high temperature, oxidation and moisture during use. In this study, we investigated the effect of this SiC layer on the tensile properties of a composite. Tensile tests of our composite samples showed the SiC layer to have no noticeable effects on its ultimate load or fracture strain, whereas it decreased the load-to-strain ratio and proportional limit. The test results were analyzed by carrying out element tests on filaments and fiber bundle samples, fracture mirror analysis of pullout fibers, and finite element analysis (FEA) of residual thermal stress around the interface.     

Tunable strength of SiCf/β-Yb2Si2O7 interface for different requirements in SiCf/SiC CMC:Inspiration from model composite investigation

Model composites consisting of Si C fiber embedded inβ-Yb₂Si₂O₇ matrix were processed by Spark Plasma Sintering method and the feasibility of tunable Si Cf/Yb₂Si₂O₇ interface in Si C-based CMCs were estimated.Weak and strengthened Si Cf/Yb₂Si₂O₇ interfaces were achieved by adjusting sintering temperatures.The indentation crack test and fiber push out experiments clearly demonstrated the different debonding mechanisms in the samples.Weak interfaces sintered at 1200 and 1250℃exhibited crack deflection at interface in indentation test.Their low debond energy at the interface,which were comparable to those of Py C or BN,satisfied the well-recognized interfacial debond and crack deflection criteria for CMCs.The interface was strengthened by atomic bonding in model composite sintered at 1450℃,leading to crack penetrating into Si C fiber and high debond energy.The strong interface may be promising in Si Cf/Si C CMC to withstand higher combustion temperature,because Yb₂Si₂O₇ will provide plastic deformation capacity,which would serve as weak interphase for crack deflection and energy dissipation.Therefore,it is possible to design the capability of Si C_f/RE₂Si₂O₇ interface for different requirements by adjusting interfacial strength or debond energy to reach optimal mechanical fuse mechanism in SiC_f/SiC CMC.     

先驱体浸渍-裂解SiC界面改性涂层对气相渗硅3D-C_f/SiC复合材料力学性能的影响

界面改性涂层对调节复合材料的力学性能起到重要作用。特别是在气相渗硅(GSI)制备C_f/SiC复合材料时,合适的界面改性涂层一方面保护C纤维不受Si反应侵蚀,另一方面调节C纤维和SiC基体的界面结合状况。通过在3D-C纤维预制件中制备先驱体浸渍-裂解(PIP)SiC涂层来进行界面改性,研究了PIP-SiC涂层对GSI C_f/SiC复合材料力学性能的影响。结果表明:无涂层改性的GSI C_f/SiC复合材料力学性能较差,呈现脆性断裂特征,其弯曲强度、弯曲模量和断裂韧性分别为87.6 MPa、56.9GPa和2.1 MPa·m~(1/2)。具有PIP-SiC界面改性涂层的C_f/SiC复合材料力学性能得到改善,PIP-SiC涂层改性后,GSI C_f/SiC复合材料的弯曲强度、弯曲模量和断裂韧性随着PIP-SiC周期数的增加而降低,PIP-SiC为1个周期制备的GSI C_f/SiC复合材料的力学性能最高,其弯曲强度、弯曲模量、断裂韧性分别为185.2 MPa、91.1GPa和5.5 MPa·m~(1/2)。PIP-SiC界面改性涂层的作用机制主要体现在载荷传递和"阻挡"Si的侵蚀2个方面。     

Determination of interfacial mechanical properties of ceramic composites by the compression of micro-pillar test specimens

A novel method to determine the fiber-matrix interfacial properties of ceramic matrix composites is proposed and evaluated; where micro-pillar samples containing inclined fiber/matrix interfaces were prepared from a SiC fiber-reinforced SiC matrix composites and then compression-tested using the nano-indentation technique. This new test method employs a simple geometry and mitigates the uncertainties associated with complex stress state in the conventional single-filament push-out method or tensile unloading–reloading hysteresis loop analysis method for the determination of interfacial properties. Based on the test results using samples with different interface orientations, the interfacial debond shear strength and the internal friction coefficient are explicitly determined and compared with values obtained by other test methods. SEM observation showed that micro compression caused an adhesive type of debonding between the fiber and the pyrolytic carbon interface. The results suggest that the debonding/failure behavior of the micro-pillars followed the Coulomb fracture criterion. The determined interfacial debond shear strength is ~100 MPa, which appears to be smaller than that determined from fiber push-out test for similar composite systems. The difference can be explained by the effect of normal stress (clamping stress) on the apparent interfacial debond shear strength.     

纤维表面涂层对SiC(f)/SiC复相陶瓷力学性能和界面结构的影响

报道了化学气相浸渍（CVI）工艺制备的SiC（f）/SiC复相陶瓷中纤维表面涂层对复合材料力学性能和显微结构的影响。SEM观察表明：C或B N表面涂层改变了SiC（f）/SiC复相陶瓷中纤维与基体间的强界面结合,使断裂过程中的界面解离和纤维拔出大大增加,与此同时材料的断裂韧性和断裂功明显提高。说明C或BN纤维表面涂层能够大大地改善SiC（f）/SiC复相陶瓷的脆性断裂行为模式。高分辨电镜的观察证实在CVI过程初期,纤维表面首先发生石墨界面相的沉积,该界面相具有明显的层状晶格条纹,而纤维表面C涂层为无定型态。