4D轴编C／C复合材料力学性能实验研究

通过宏观力学实验研究了4D轴编C／C复合材料的各向拉伸、压缩和剪切性能。采用ARAMIS非接触式应变测试系统有效地解决了常规测试中应变片和试样变形不协调的问题。结果表明：4D轴编C／C复合材料在拉伸、压缩和剪切时表现出较强的各向异性,具有双模量和非线性特征,径向拉伸表现为裂纹分层扩展,轴向拉伸表现为炭棒拔出,压缩时延性...     

弯曲疲劳后4D-C/C复合材料的抗弯强度及热膨胀性能(英文)

采用液相浸渍炭化技术,在压力为75MPa下制备出4D-C/C复合材料,并进行高温热处理。研究静态和动态加载条件下,材料沿厚度方向的弯曲性能及断裂行为。结果表明,循环次数达到10×105次、频率为10 Hz时,材料的临界弯曲疲劳极限是静态弯曲强度的80%。静态弯曲加载情况下,C/C复合材料失效机制取决于试样底层炭纤维的取向。循环疲劳载荷作用下,其失效机制包括基体开裂、纤维-基体界面弱化及纤维断裂。复合材料在循环加载过程中界面结合强度降低,并释放内应力,故增强了纤维拔出以及复合材料的假塑性,疲劳加载后其剩余弯曲强度增加10%左右,而模量降低。疲劳载荷引起材料基体缺陷和裂纹数量的增加及纤维断裂,削弱了长度方向上的热膨胀,使材料热膨胀系数降低。     

3D-C/SiC复合材料拉伸蠕变损伤和蠕变机理

对3D-C/SiC复合材料进行拉伸蠕变试验,蠕变进行一段时间后,用扫描电子显微镜(SEM)观察试样表面的变化,同时测量试样的共振频率.结果表明,3D-C/SiC除通常CMC所产生的蠕变损伤外,纤维束滑动,纤维束之间的夹角变化,孔隙变形,部分孔隙表面空间位置改变,孔隙表面产生基体微裂纹,损伤在纤维束交叉处更为集中,这些可作为3D-C/SiC蠕变变形的独特机理.电阻和模量的相对变化与蠕变曲线相似,因此电阻和模量都可表征C/SiC材料的蠕变损伤,作为损伤变量.该材料的蠕变属于损伤引起.     

先驱体浸渍裂解C/SiCN复合材料的拉伸行为与基体开裂机制

采用先驱体浸渍裂解法制备陶瓷基复合材料过程中会形成基体裂纹和孔隙, 基体开裂和裂纹演化机制是工艺设计和性能优化的依据。本研究采用真空旋转浸渍-裂解法制备了无界面相的纤维束C/SiCN复合材料, 分析了该材料的拉伸性能和基体裂纹增殖现象, 讨论了浸渍裂解次数和热处理温度对基体裂纹的影响规律。研究结果表明: 当热处理温度为1000~1400 ℃时, 该复合材料的化学组成变化较小; 热处理温度达到1600 ℃时, 先驱体转化的SiCN基体分解, C含量降低, SiC含量升高。随浸渍裂解次数由1次增加到4次, 该复合材料的平均拉伸强度分别提升14.19%、38.83%和63.47%, 同时基体裂纹间距和裂纹开口距离均逐渐减小, 基体纤维结合增强, 断口纤维拔出减少。热处理温度从1000 ℃升高到1400 ℃, C/SiCN拉伸强度缓慢增大; 热处理温度为1600 ℃时, SiCN基体由无定形的SiC_xN_4-x四面体向SiC晶体转变, 基体与纤维脱粘, 二者结合强度降低, 同时基体体积收缩使C纤维损伤, 导致该复合材料拉伸强度陡然下降30.0%。     

径棒法编织C/C复合材料高温拉伸性能研究

采用化学气相沉积、沥青浸渍-高压碳化混合致密工艺向径棒法编织的预制体内引入基体碳,实现高密度(≥1.94g/cm3)炭/炭复合材料制备。利用快速通电加热测试技术,模拟C/C复合材料的高温工作环境,研究不同温度下材料的环向拉伸性能。结果表明:在2 300℃时,材料拉伸强度最大(80.3 MPa),断裂应变随着温度的升高而增加。采用扫描电镜对试样及断口形貌进行观察,发现测试温度、机加损伤及试样过渡区应力集中影响材料断裂特征。温度为1 800℃、2 300℃时材料在过渡区断裂;温度为2 800℃时,材料在标距区发生破坏,纤维与基体界面结合强度低,纤维拔出多,表现出假塑性断裂特征。     

2D-C/ SiC 复合材料的宏观拉压特性和失效模式

通过拉伸、压缩实验, 从宏观上研究了平纹编织C/ SiC 复合材料在简单载荷作用下模量、残余应变及泊松比的变化。通过断口观察, 分析了材料在面内拉、压载荷作用下的损伤与失效模式。实验结果表明, 拉伸载荷作用下, 材料在低应力就开始损伤。0°纤维束表面基体开裂和层间裂纹是主要损伤形式。损伤后, 随着应力增加, 拉伸卸载模量、泊松比线性减小, 残余应变增加; 压缩应力-应变基本呈直线关系, 模量、泊松比基本不变。拉伸破坏表现为韧性断裂, 断裂机理为分层后0°纤维束的断裂、携带90°纤维束拔出; 压缩破坏形成一个与加载方向成13°的断裂平面, 破坏机理为层间裂纹、0°/ 90°纤维束之间裂纹和90°纤维束内裂纹的产生和迅速扩展、最后0°纤维束剪切断裂。      

整体毡碳/碳复合材料的高温剪切性能研究

运用双槽口剪切试验方法测试了碳纤维增强碳基复合材料(C/C)在室温、700℃、1000℃、1400℃下的剪切强度,并用扫描电子显微镜(SEM)观察了材料的原始组织形貌和断口微观形貌。结果表明:材料的剪切强度在一定范围内随温度的升高而增加,材料Z向的剪切强度优于XY向。通过SEM观察分析可知,材料XY向和Z向纤维的含量明显不同;室温下,C/C复合材料的破坏形式有纤维拔出及断裂,而高温下,失效形式主要为纤维的拔出、纤维/基体界面脱粘等。     

2D-C/C复合材料及其石墨化制品烧蚀特性分析

以液化石油气为碳源,2D炭纤维织物为基体,通过1000℃~1100℃沉积热解炭,制备了沉积态2D-C/C复合材料。通过对沉积态2D-C/C复合材料在2800℃热处理10h制备了石墨态2D-C/C复合材料。采用小型发动机烧蚀实验对两种复合材料的烧蚀性能进行了测试和评价;通过比较两种复合材料的孔隙分布、基体和纤维的结合强度以及热导率,解释了它们不同的烧蚀特性和烧蚀机理。结果表明:沉积态2D-C/C复合材料由于孔隙分布少、基体和纤维结合强度大、面间热导小,烧蚀主要由热化学反应(氧化)控制,烧蚀表面平整,烧蚀率为0.033mm/s。石墨态2D-C/C复合材料由于孔隙分布多、基体和纤维结合强度小,烧蚀主要由氧化和机械剥蚀控制,烧蚀表面出现烧蚀坑,烧蚀率为0.046mm/s。     

基于改进遗传算法的C/SiC拉伸损伤声发射模式识别

采用层次聚类及基于改进遗传算法的无监督模式识别方法,对2D-C/SiC复合材料常温拉伸试验过程的声发射数据进行分析,结合试样断口的扫描电镜(SEM)照片,得到拉伸过程中5类损伤模式及其典型声发射特征参数。通过对各类损伤的能量分布、累计事件数和累计能量的分析,研究C/SiC复合材料的损伤演化过程,发现其过程可分为基体微裂纹和界面失效为主的初始损伤阶段、基体微裂纹停滞导致层间剥离及纤维失效占主导地位的裂纹饱和阶段、基体长裂纹和界面失效为主的损伤积累发展阶段和纤维束大量失效的宏观断裂阶段。     

三维编织SiC/SiC复合材料拉伸和弯曲损伤机制

为了研究三维编织SiC/SiC复合材料损伤机制,开展了室温条件下的单调拉伸和三点弯曲试验。实验前,利用CT扫描手段,明确了三维编织SiC/SiC复合材料试样的编织组织形态。对拉伸和三点弯曲试样的微观分析表明:原生孔洞和微裂纹导致了材料在单调拉伸过程中形成局部应力集中,随着拉伸载荷的增大,基体的横向开裂和纤维束间纵向层间裂纹逐渐演化形成纤维内部裂纹,导致材料最终的脆性断裂失效;在三点弯载荷作用下,表现为剪切、拉压共生的多耦合破坏模式,拉应力一侧首先发生失效,随后在中性面处发生剪切破坏,紧接着失效迅速向上下两侧扩展,直至截面在整个厚度方向发生失效;断口与纤维束的走向相关性很大,裂纹基本上沿着纤维束之间的界面进行扩展,导致最终失效未发生在理论失效位置处。      

短切炭纤维增强沥青基C/C复合材料的组织特征

利用新型、高效的模压半炭化成型工艺，在大气环境下制备出了短切炭纤维增强沥青基C／C复合材料制品，并借助光学显做镜和扫描电镜对其微观组织和断口形貌进行了观察。通过分析，解释了短切炭纤维增强沥青基C／C复合材料中炭纤维损伤的形成机制，提出了作为增强体相的短切炭纤维和焦炭颗粒与基体炭之间独特的界而结构模型。研究还表明：复合材料中明显存在着基体相和颗粒相一基体相的显微结构不仅呈层片状，而且层片状的结构好像数层桔子皮，将颗粒相包裹起来，这种“桔皮包裹”式的结构与炭纤维表面的POG结构基本相似。     

短切炭纤维增强沥青基C/C复合材料的力学性能

利用模压半炭化成型工艺在大气环境下制备出了短切炭纤维增强沥青基C／C复合材料（简称SCFRC）。研究了短切炭纤维的体积分数对SCFRC材料的体积密度和力学性能的影响规律。借助光学显微镜和扫描电镜对其微观组织和断口形貌进行了观察，分析了短切炭纤维对SCFRC材料的增强机制。结果表明，当短切炭纤维的体积分数由0％增大到11．8％时，SCFRC材料的力学性能随之呈线性增加；短切炭纤维增强SCFRC材料的机制主要有裂纹偏转效应、桥联效应以及脱粘和拔出效应。     

Kinetics of chemical vapor infiltration of carbon nanofiber-reinforced carbon/carbon composites

Preforms containing 0, 5, 10, 15 and 20 wt.% carbon nanofibers (CNFs) were fabricated by spreading layers of carbon cloth, and infiltrated by using the technique of isothermal chemical vapor infiltration (ICVI) at the temperature of 1100 °C under the total pressure of 1 kPa and with the flow of the mixture of propane/nitrogen in a ratio of 13:1. The infiltration rates increased with the rising of CNF content, and after 580 h of infiltration, the achievable degree of pore filling was the highest when the CNF content was 5 wt.%, but the composite could not be densified efficiently as the CNF content ranged from 10 to 20 wt.%. An analysis of the results, based on the effective diffusion coefficient and on the in-pore deposition rates, shows that the CNFs, due to their higher aspect ratio, accelerate overgrowth at pore entrances and thus lead to incomplete pore filling.     

Hierarchical carbon nanostructure design: ultra-long carbon nanofibers decorated with carbon nanotubes

Hierarchical carbon nanostructures based on ultra-long carbon nanofibers (CNF) decorated with carbon nanotubes (CNT) have been prepared using plasma processes. The nickel/carbon composite nanofibers, used as a support for the growth of CNT, were deposited on nanopatterned silicon substrate by a hybrid plasma process, combining magnetron sputtering and plasma-enhanced chemical vapor deposition (PECVD). Transmission electron microscopy revealed the presence of spherical nanoparticles randomly dispersed within the carbon nanofibers. The nickel nanoparticles have been used as a catalyst to initiate the growth of CNT by PECVD at 600°C. After the growth of CNT onto the ultra-long CNF, SEM imaging revealed the formation of hierarchical carbon nanostructures which consist of CNF sheathed with CNTs. Furthermore, we demonstrate that reducing the growth temperature of CNT to less than 500°C leads to the formation of carbon nanowalls on the CNF instead of CNT. This simple fabrication method allows an easy preparation of hierarchical carbon nanostructures over a large surface area, as well as a simple manipulation of such material in order to integrate it into nanodevices.     

Diamond formation on carbon/carbon composite

A carbon/carbon composite was used as substrate for low-pressure diamond deposition. To enhanced diamond nucleation on carbon/carbon composites, a total of ten surface preparation methods have been investigated. These methods involved the use of atomic hydrogen etching, mechanical polishing, sonication, or coating. Diamond nucleation was found to occur on either the defects of the carbon/carbon composite substrates or diamond particulate left on the substrates. The defects were created primarily by atomic hydrogen etching during the coating process. Seeding with diamond powders was performed by dip coating, sonication, or spray-coating processes. It was found that these seeding processes resulted in excellent nucleation of diamond.     

Graphitization behaviour of carbon fibre-glassy carbon composites

Carbon fibre-carbon composites were fabricated by aligning PAN-based carbon fibre unidirectionally in furfuryl alcohol resin char. The graphitization behaviour was investigated by an X-ray diffraction technique and by the measurement of magnetoresistance. The time-temperature superimposition study for interlayer spacing resulted in an activation energy of 242±35 kcal mol⁻¹. The kinetic study on magnetoresistance agreed with the result of X-ray measurement. The activation energy is that for the graphitization of the layer structure formed in the glassy carbon matrix of the composites. The graphitization mechanism of the layer structure is the same as that of soft carbons.     

Mesoscale evolution of non-graphitizing pyrolytic carbon in aligned carbon nanotube carbon matrix nanocomposites

Polymer-derived pyrolytic carbons (PyCs) are highly desirable building blocks for high-strength low-density ceramic meta-materials, and reinforcement with nanofibers is of interest to address brittleness and tailor multi-functional properties. The properties of carbon nanotubes (CNTs) make them leading candidates for nanocomposite reinforcement, but how CNT confinement influences the structural evolution of the PyC matrix is unknown. Here, the influence of aligned CNT proximity interactions on nano- and mesoscale structural evolution of phenol-formaldehyde-derived PyCs is established as a function of pyrolysis temperature (\(T_{\mathrm {p}}\)) using X-ray diffraction, Raman spectroscopy, and Fourier transform infrared spectroscopy. Aligned CNT PyC matrix nanocomposites are found to evolve faster at the mesoscale by plateauing in crystallite size at \(T_{\mathrm {p}}\) \(\sim\)800 \(^{\circ }\hbox {C}\), which is more than \(200\,\,^{\circ }\hbox {C}\) below that of unconfined PyCs. Since the aligned CNTs used here exhibit \(\sim\)80 nm average separations and \(\sim\)8 nm diameters, confinement effects are surprisingly not found to influence PyC structure on the atomic-scale at \(T_{\mathrm {p}}\) \(\le \)1400 \(^{\circ }\hbox {C}\). Since CNT confinement could lead to anisotropic crystallite growth in PyCs synthesized below \(\sim\)1000 \(^{\circ }\hbox {C}\), and recent modeling indicates that more slender crystallites increase PyC hardness, these results inform fabrication of PyC-based meta-materials with unrivaled specific mechanical properties.     

Horizontally oriented carbon nanotubes coated with nanocrystalline carbon

Single-walled carbon nanotubes (CNTs) and multi-walled CNTs of length 2-5 mm were grown from Fe/Mo nanoparticles and Fe thin film catalyst, respectively, by thermal chemical vapor deposition. Following CNT growth, the CNTs were in-situ coated with nanocrystalline carbon shells of thickness 100-1500 nm. Horizontally oriented CNTs with carbon shells in the direction of the feeding gas were visible under a regular optical microscope. They were easily manipulated by optical manipulators, and CNT probes can thus be fabricated.     

Co-synthesis of single-walled carbon nanotubes and carbon fibers

A new vertical floating catalytic technique is developed and used to prepare both single-walled carbon nanotubes (SWNTs) and carbon fibers (CFs). Scanning electron microscopy (SEM) observation shows a clear separation of these two materials. Thin films of SWNTs can be peeled easily from the CF substrate which just acts as a catalyst support for the SWNT growth. The production process is also semicontinuous, resulting in a yield of ∼1.0 g h⁻¹ of SWNTs film with high purity. Structure and vibrational properties of these materials are investigated by electron microscopy and Raman spectroscopy, respectively.