微观结构对中间相沥青基炭/炭复合材料力学性能的影响

借助偏光显微镜、扫描电镜、透射电镜以及力学性能测试研究了微观结构对中间相沥青基炭/炭复合材料力学性能的影响. 结果表明: 基体炭在偏光显微镜下呈现出光学各向异性, 在SEM和TEM下呈片层条带状结构. 基体炭与纤维之间的界面不连续, 为“裂纹型”界面. 材料受载破坏时裂纹通过改变扩展路径而延缓其扩展速度, 在纤维-基体界面处以及基体炭层片之间引起滑移, 在断口形貌上体现出断裂台阶适中且与纤维拔出交替进行, 表现出韧性破坏的断裂特征. 材料具有较高的力学性能, 抗弯强度达到257MPa, 断裂韧性达到11.4MPa·m ^1/2.     

微观组织结构对C/C复合材料力学行为的影响

采用快速化学液相气化渗透法制备了2D-C/C复合材料,沉积温度为1200-1250℃, 系统压力约0.1MPa.利用偏光显微镜及扫描电子显微镜观察了不同沉积温度制备的基体热解碳的微观组织结构及断口形貌.实验结果表明,1200℃沉积的基体热解碳中粗糙层组织占大多数,其弯曲强度较高、韧性较低; 1250℃的基体热解碳呈现为光学各向异性程度不同的光滑层/粗糙层交替层状组织,其弯曲强度较低、韧性较高,具有非脆性断裂行为.不同微观结构的材料具有不同的强度及断裂模式,除了纤维/基体间界面结合强度不同外,不同温度沉积得到的热解碳微观结构的不同引起裂纹在不同微观结构碳层内的扩展阻力也会不同.此外,裂纹在光滑层/粗糙层界面处的偏转会导致断裂面的高低不平,从而使后者韧性增强.     

沥青过渡层对C/C复合材料力学性能的影响

在2D碳／碳（C／C）复合材料的碳纤维与基体热解碳间引入中间相沥青做过渡层，研究了中间相沥青的引入对C／C复合材料力学性能的影响．结果表明，与没有过渡层，普通沥青做过渡层、中间相沥青做过渡层的三类C／C复合材料比较．采用沥青做过渡层可以提高复合材料的力学性能，采用中间相沥青做过渡层制备的C／C复合材料的弯曲强度比采用普通沥青做过渡层提高44％，剪切强度提高15％．中间相沥青的引入可以使碳纤维束间和束内的结合强度不同，从而使基体断裂产生的裂纹扩散时发生偏转，复合材料的强度和韧性同时得到提高．     

Mechanical behavior of SiCf/SiC composites with alternating PyC/SiC multilayer interphases

In order to tailor the fiber–matrix interface of continuous silicon carbide fiber reinforced silicon carbide (SiC_f/SiC) composites for improved fracture toughness, alternating pyrolytic carbon/silicon carbide (PyC/SiC) multilayer coatings were applied to the KD-I SiC fibers using chemical vapor deposition (CVD) method. Three dimensional (3D) KD-I SiC_f/SiC composites reinforced by these coated fibers were fabricated using a precursor infiltration and pyrolysis (PIP) process. The interfacial characteristics were determined by the fiber push-out test and microstructural examination using scanning electron microscopy (SEM). The effect of interface coatings on composite mechanical properties was evaluated by single-edge notched beam (SENB) test and three-point bending test. The results indicate that the PyC/SiC multilayer coatings led to an optimum interfacial bonding between fibers and matrix and greatly improved the fracture toughness of the composites.     

具有中间相沥青过渡层的炭/炭复合材料的微观结构与力学性能

采用液相浸渍-炭化和CVI复合工艺, 制备出在炭纤维和热解炭之间具有中间相沥青过渡层的炭/炭复合材料, 借助偏光显微镜、扫描电镜、透射电镜以及力学性能测试研究了所制备的炭/炭复合材料的微观结构与力学性能. 结果表明: 在偏光显微镜下中间相沥青炭的光学活性高于热解炭的光学活性, 中间相沥青炭在SEM和TEM下均呈片层条带状结构, 热解炭在SEM下呈“皱褶状”片层结构, 在TEM下为粒状结构; 在HRTEM下, 中间相沥青炭、热解炭和炭纤维的晶化程度依次降低. 在加载过程中, 材料内部多层次的界面通过改变裂纹扩展路径而延缓其扩展速度, 在断口形貌上体现出锯齿状的断裂形式, 纤维拔出长度适中, 材料表现出韧性破坏的断裂特征. 材料具有较高的力学性能, 抗弯强度达到244MPa, 断裂韧性达到9.7MPa·m^1/2.     

Microstructure and thermal conductivity of carbon/carbon composites containing zirconium carbide

Carbon/carbon (C/C) composites containing zirconium carbide (ZrC) were prepared by a novel method. Carbon fiber felt with addition of zirconia was prepared by a microwave-hydrothermal reaction, followed by densification and graphitization. The crystalline structure of the pyrolytic carbon and morphology of the composites were investigated by X-ray diffraction, Raman spectrascope, polarized light microscope, and scanning electron microscopy. Results show that the ZrC grains with sub-micron size present a homogeneous distribution in carbon matrix. The degree of order of the pyrolytic carbon matrix is decreased due to adding ZrC into the C/C composites. Graphitization degree of the C/C composites is decreased by the addition of ZrC. ZrC grains uniformly embedded in the pyrolytic carbon matrix act as pinning particles blocking the conversion of disordered to ordered structure during graphitization. Thermal conductivity is higher in the C/C composites containing ZrC, which is attributed to the increased phonon-defect interaction produced by the thermal motion of the CO in the micropores and gaps of the composites.     

两种双基体C/C复合材料的微观结构与力学性能

借助偏光显微镜、扫描电镜以及力学性能测试研究了两种双基体C/C复合材料的微观结构与力学性能。结果表明:基体碳在偏光显微镜下呈现出热解碳的光滑层组织,沥青碳的各向同性、镶嵌和流域组织。在SEM下普通沥青碳为"葡萄状"结构,中间相沥青碳为片层条带状结构。具有多层次界面结构的材料可以提高材料的弯曲强度,改善材料的断裂韧度,两种材料在载荷-位移曲线中载荷为台阶式下降,呈现出假塑性断裂特征。材料A和材料B的弯曲强度分别为206.68,243.66MPa,断裂韧度分别为8.06,9.66MPa·m1/2,材料B的弯曲强度、断裂韧度均优于材料A。     

Effect of matrix sub-layer interfacial fracture on residual strength improvement of the fatigued carbon/carbon composites

In the present study, flexural behavior of carbon fiber reinforced pyrolytic carbon matrix composites (C/C composites) before and after fatigue tests had been studied. The results showed that the residual flexural strengths of the samples had been improved after fatigue tests, and the fracture mechanisms of the original and post-fatigue specimens had some differences. Fracture mechanism of the original specimens could be described as fiber/matrix interfacial de-bonding, and the dominant damage of the post-fatigue specimens could be regarded as pyrolytic carbon sub-layers’ step-delamination. The degradation of matrix sub-layer interfacial bonding strength was beneficial to improve the mechanical properties of C/C composites.     

C/SiC/Si-Mo-Cr复合涂层碳/碳复合材料力学性能研究

采用包埋法和涂刷法在碳/碳复合材料表面制备了一种新型的C/SiC/Si-Mo-Cr复合高温抗氧化涂层. 借助XRD和SEM等测试手段对所制备复合涂层的微观结构进行了表征, 采用三点弯曲试验研究了涂层处理及热震试验对碳/碳复合材料力学性能的影响规律. 结果表明: 制备的多相涂层结构致密, 涂层后碳/碳复合材料弯曲强度有所增大, 断裂特征由假塑性向脆性转变. 涂层试样经1500℃至室温20次热震后, 涂层试样的弯曲强度降低, 塑性增强.     

Veränderung des elektrochemischen Korrosionsverhaltens und der mechanischen Eigenschaften von C/Al-Verbunden durch Faserbeschichtungen aus SiC und pyrolytischem Kohlenstoff

Changes of the electrochemical corrosion behavior and the mechanical properties of C/Al-composites due to SiC and pyrolytic carbon fiber coatings The following contribution describes the modification of the electrochemical and mechanical behavior of carbon fiber reinforced pure aluminum (C/Al-composite) due to two different fiber coatings. Tests include potentiodynamic corrosion tests, Transmission electron microscopy, bending tests and single fiber-“push in”-tests. The potentiodynamic corrosion tests were carried out in 3,5 wt.% NaCl solution. The results give evidence of a considerable decrease of the corrosion resistance of the C/Al-composites due to the application of the pyrolytic fiber coating. The SiC coating improves the corrosion resistance of the composite. However, the mechanical properties of the composites were harmed by the SiC coating. The pyrolytic carbon coating leads to a remarkable energy dissipation due to “stick-slip” effects on the interface under load. Consequently, the application of suitable multilayers of pyrolytic carbon and SiC fiber coatings could result in improved electrochemical and optimized mechanical properties of the C/Al-composite.     

2D C/C复合材料微观结构与力学性能的研究

采用等温化学气相渗透方法,通过调整沉积工艺,制备了具有不同微观组织结构的2D C/C复合材料.利用偏光显微镜(PLM)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)结合选区电子衍射(SAED),研究了热解炭基体微观组织结构,借助万能试验机测试了材料的三点弯曲性能.结果表明:层状高织构(HT)热解炭基体占优时C/C复合材料表现为假塑性断裂;扁平片状中织构(MT)热解炭与颗粒状各向同性层热解炭(ISO)有利于提高材料的弯曲强度;HT基体与炭纤维界面结合良好,界面处不存在非HT织构,但取向角(OA)略有增大.     

Shear strength and fracture toughness of carbon fibre/epoxy interface: effect of surface treatment

Textile-reinforced composites have become increasingly attractive as protection materials for various applications, including sports. In such applications it is crucial to maintain both strong adhesion at fibre–matrix interface and high interfacial fracture toughness, which influence mechanical performance of composites as well as their energy-absorption capacity. Surface treatment of reinforcing fibres has been widely used to achieve satisfactory fibre–matrix adhesion. However, most studies till date focused on the overall composite performance rather than on the interface properties of a single fibre/epoxy system. In this study, carbon fibres were treated by mixed acids for different durations, and resulting adhesion strength at the interface between them and epoxy resin as well as their tensile strength were measured in a microbond and microtensile tests, respectively. The interfacial fracture toughness was also analysed. The results show that after an optimum 15–30 min surface treatment, both interfacial shear strength and fracture toughness of the interface were improved alongside with an increased tensile strength of single fibre. However, a prolonged surface treatment resulted in a reduction of both fibre tensile strength and fracture toughness of the interface due to induced surface damage.     

The effect of zirconium addition on the microstructure and properties of chopped carbon fiber/carbon composites

Carbon/carbon composites containing zirconium were prepared using chopped carbon fiber, mesophase pitch and Zr powder by the traditional process including molding, carbonization, densification and graphitization. The influence of Zr on the microstructure and properties of the composites were investigated. Results show that Zr can improve the interface bonding, promote more perfect and larger crystallites and enhance the conductive/mechanical properties of the composites. The high in-plane thermal conductivity of 464 W/(m K) and excellent bending strength of 83.6 MPa was obtained for a Zr content of 13.9 wt% at heat treatment temperature(HTT) of 2500 °C. However the conductive/mechanical properties of the composites decrease dramatically for an higher HTT of 3000 °C. SEM micrograph of the fracture surface for the composites shows that lower disorder crystallite arrangement of fiber and carbon matrix come into being in the composites during HTT of 3000 °C, which should be responsible for the low properties. Correlation between the content of Zr and the microstructure and properties are discussed.     

高压浸渍-炭化制备炭/炭复合材料的组织结构

为研究高压浸渍-炭化制备的炭/炭复合材料的组织结构,以1 K PAN基高强度炭纤维为增强体,以调制中温煤沥青为基体前驱体,采用超高压浸渍-炭化工艺制备出2.5D沥青基炭/炭复合材料.采用偏光显微镜及SEM电镜对材料内部的组织形态进行了观察.研究表明:以中温沥青为基体前驱体所制备的炭/炭复合材料,在纤维束内,由于纤维之间的孔隙较小,形成的基体组织主要为镶嵌组织;而在纤维束之间,由于空间较大,出现的基体组织既有镶嵌型组织,也有域型组织.在沥青基炭基体中,有孔洞、裂纹、沟槽等缺陷.     

Structure-property relations for silicon nitride matrix composites reinforced with pyrolytic carbon pre-coated Hi-Nicalon fibers

Si₃N₄ matrix composites reinforced with pyrolytic carbon pre-coated Hi-Nicalon (SiC) fibers, were studied using tensile testing and transmission electron microscopy. Three types of samples were evaluated all with a nominal coating thickness of 200 nm. The composites were densified by hot pressing at 1550 °C (type I and II) and at 1600 °C (type III). The fibers were coated with pyrolytic carbon via CVD with identical (sample I) and opposite (samples II and III) directions of the gas flow and of the fiber movement through the reactor. Tensile testing indicated for the three sample types respectively: brittle behaviour with huge pull out of the fibers, pseudo-plastic behaviour and brittle behaviour with little pull out. TEM indicated for the three sample types debonding typically at the fiber/coating interface, at the coating/matrix interface and in the coating, respectively. The relation between processing, structure, particularly of the coating and its interfaces with the matrix and the fibers and mechanical properties is addressed.     

C／C复合材料的显微结构及其与工艺、性能的关系

对化学气相渗透（CVI）C／C复合材料在偏振光下的显微结构（偏光显微结构）类型、结构的形貌特征及对应炭的基本物理性能、材料的制备工艺参数－结构－性能之间的关系进行了综述。C／C复合材料具有三种基本偏光显微结构,即RL、SL和ISO。这三种基本偏光结构的炭对应于不同的形貌特征,可从消光十字形、旋光性、光学反射性、生长特征、表面织构、择优取向性和环形裂纹等特征将其分辨出来。工艺参数对沉积炭偏光显微结构的影响没有一成不变的规律可循,影响因素除了温度、压力、气体成分、气体流速外,还与炉子的几何尺寸及试样的堆积尺寸有关,对不同的CVI体系,都应当摸索出一套适合其运行的最佳工艺参数。C／C复合材料的偏光显微结构与材料的性能有着密切的联系,不同的结构下,材料的物理性能、力学性能和热性能都表现出明显的差异。通过归纳与分析,获得了对C／C复合材料偏光显微结构全面、系统的认识,明确了它在C／C复合材料研究中的重要性,为制备具有单一、均匀偏光显微结构及所需性能的C／C复合材料指明了方向。     

双基体炭/炭复合材料的微观结构与力学性能

借助偏光显微镜、扫描电镜,透射电镜以及力学性能测试研究了微观结构对双基体炭/炭复合材料力学性能的影响.结果表明:基体炭在偏光显微镜下呈现光学各向异性,材料内部形成多层次的界面结构,热解炭呈现"皱褶状"片层结构,中间相沥青炭呈现片层条带状结构,基体炭片层的走向基本上平行于纤维轴向.材料受载破坏时裂纹通过改变扩展路径而延缓其扩展速度,在纤维-基体界面处以及基体炭片层之间引起滑移,在断口形貌上体现出锯齿状的断裂形式,材料具有韧性断裂的特征,抗弯强度最高可达223MPa.     

Comparison of chemical vapor deposition and chemical grafting for improving the mechanical properties of carbon fiber/epoxy composites with multi-wall carbon nanotubes

By engineering the fiber/matrix interface, the properties of the composite can be changed significantly. In this work, we increased the effective surface area of the fiber/matrix interface, to facilitate additional stress transfer between fibers and matrix, by grafting carbon nanotubes on to carbon fibers (in the form of carbon fabric) by two different methods: (1) chemical vapor deposition (CVD) method and (2) a purely chemical method. With the CVD process, carbon nanotubes (CNT) were directly grown on carbon fiber substrate using chemical vapors. For the chemical method, CNT with carboxyl groups were grafted on functionalized carbon fiber via a chemical reaction. The morphology of CNT/carbon fibers was examined by scanning electron microscope (SEM) which revealed uniform coverage of carbon fibers with CNT in both of CVD method and chemical grafting method. CNT-grafted woven carbon fibers were used to make carbon/epoxy composites, and their mechanical properties were measured using three-point bending and tension tests which showed that those with CNT-grafted carbon fiber reinforcements using the CVD process has 11 % higher tensile strength compared to those containing carbon fibers modified with the chemical method. Also, composites with CNT-grafted carbon fibers with chemical method showed 20 % higher tensile strength compared to composites with unmodified carbon fibers. The results of tensile test revealed that both CVD and chemical grafting could significantly improve the mechanical properties of the carbon fiber composites.     

Enhancing both strength and toughness of carbon/carbon composites by heat-treated interface modification

A simple method to increase both strength and toughness of carbon/carbon (C/C) composites is presented. This method is based on the heat treatment of the pre-deposited thin carbon coating, leading to the formation of more orderly pyrolytic carbon (PyC) as a functional interlayer between fiber and matrix that could optimize the interfacial sliding strength in C/C composites. Effects of such a heat-treated PyC layers on the microstructure, tensile strength and fracture behavior of unidirectional C/C composites were investigated. Results showed that although the in-situ fiber strength was deteriorated after the introduction of interfacial layer, tensile strength of the specimen was greatly improved by 38.5% compared with pure C/C composites without any treatment. The interfacial sliding stress sharply decreased, which was interpreted from finite element analysis and verified by Raman spectra. Therefore, the fracture behavior was changed from brittle fracture to multiple-matrix cracking induced non-linear mechanical behavior. Finally, the ultimate strength can be predicted by different models according to the interfacial sliding stress. Our research would provide a meaningful way to improve both strength and toughness of C/C composites.     

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.