C／C坯体对RMI C／C—SiC复合材料组织的影响

以PAN基炭纤维（Cf）针刺整体毡为预制体，用化学气相渗透（CVI）、浸渍炭化（IC）方法制备了不同炭纤维增强炭基体的多孔C／C坯体，采用反应熔渗（RMI）法制备C／C—SiC复合材料，研究了渗Si前后坯体的密度和组织结构。结果表明：不同C／C坯体反应溶渗硅后复合材料的物相组成为SiC相、C相及单质Si相；密度低的坯体熔融渗硅后密度增加较多；密度的增加与开口孔隙度并不是单调增加的关系，IC处理的坯体开口孔隙度低，但渗硅后复合材料的密度增加较多；IC坯体中分布分散的树脂C易与熔渗Si反应，CVI坯体中的热解C仅表层与熔渗Si反应，在Cf和SiC之间有热解C存在；坯体密度相同时，IC处理的坯体中SiC量较多，单质Si相含量少且分散较好，而CVI坯体中SiC量较少，单质Si相的量较多；制备方法相同时，高密度的C／C坯体，渗硅后C相较多。     

Rapid fabrication of C/C/SiC composite by PIP of HMDS

The C/C/SiC composite was fabricated within several days by the method of precursor impregnation and pyrolysis (PIP) using hexamethyldisilazane (HMDS) as the precursor. The carbon fiber plates, woven and punctured with two-dimensional orthogonal continuous carbon bundle and short carbon fiber, were used as the reinforced preforms. The characters of the C/C/SiC composite were analyzed using XRD, EDS and SEM, and three-point-bending test. The results indicated that pyrolyzed substance of the precursor contained excessive carbon, followed by silicon, and a small amount of nitrogen. There were micro-cracks on the massive matrix. The phase composition was difficult to distinguish, primarily considered as the Si–C–N composite. The structure of C/C/SiC was dense and homogeneous with some pores whose sizes were less than 5 μm between fibers and less than 100 μm between the carbon fiber bundles, respectively.

Fiber pull-out was observed on the bending fracture surface. The stress–strain curve of both at room temperature and 1300 °C appeared ascending zigzag. Flexural strength was 150 MPa at 1300 °C, higher than 121 MPa at room temperature.     

Densification Behavior and Performances of C/C Composites Derived from Various Carbon Matrix Precursors

Three types of carbon/carbon (C/C) composites were manufactured by densifying the needled carbon fiber preform through resin and pitch impregnation/carbonization repeatedly, as well as propylene pyrolysis by chemical vapor infiltration plus carbonization after the resin impregnation/carbonization. The densification behavior and performances (involving electric, thermal, and mechanical properties, as well as impurity) of the C/C composites were investigated systematically. The results show that besides the processing and testing conditions, the electric resistivity, thermal conductivity (TC), coefficient of thermal expansion (CTE), strength, and fracture, as well as impurity content and composition of the C/C composites were closely related to the fiber orientation, interfacial bonding between carbon fiber and carbon matrix, material characteristics of the three precursors and the resulting matrix carbons. In particular, the resin-carbon matrix C/C (RC/C) composites had the highest electric resistivity, tensile, and flexural strength, as well as impurity content. Meanwhile, the pitch-carbon matrix C/C (PC/C) composites possessed the highest TC and CTE in the parallel and vertical direction. And most of the performances of pyro-carbon/resin carbon matrix C/C composites were between those of the RC/C and PC/C composites except the impurity content.     

基体碳对C/CF/Cu复合材料的影响

采用树脂碳化和碳气相沉积相结合的方法制备了碳／碳纤维（C／CF）先驱丝，用压力浸渗凝固成形方法制备了碳／碳纤维／铜（C／CF／Cu）复合材料，借助于扫描电镜下复合材料界面和相分布观察，以及显微硬度和滑动摩擦磨损测试，探讨了基体碳（树脂碳化碳和沉积碳）对C／CF／Cu复合材料成形、显微硬度及摩擦磨损的影响。结果表明，碳化和碳气相沉积处理的C／CF先驱丝相对致密，并阻碍铜液的压力浸渗成形，但该先驱丝硬度高于碳化处理的C／CF先驱丝。碳化和碳气相沉积处理的C／CF／Cu复合材料滑动摩擦磨损耐磨性高于纯铜，而且滑动摩擦因数也高于纯铜。证明C／CF／Cu复合材料是一种具有摩阻功能的复合材料。     

C/CF/Cu复合材料界面和抗拉强度研究

采用树脂碳化方法制备了碳/碳纤维(C/CF)先驱丝,用压力浸渗凝固成型方法制备了碳/碳纤维/铜(C/CF/Cu)复合材料,借助抗拉强度测试及扫描电镜下复合材料界面和相组成物分布观察,探讨了C、CF和Cu三组元复合界面特性以及碳纤维丝类型和C/CF先驱丝体积分数对C/CF/Cu复合材料抗拉强度的影响.结果表明,C/CF/Cu复合材料的微观界面是碳纤维单丝-树脂碳化碳-铜双复合界面,此界面属于无化学反应的弱复合界面,铜对C/CF先驱丝的机械锁紧力是提高界面强度和复合材料强度的关键因素.当凝固成型压力为28.5MPa时,1k碳纤维丝的C/CF先驱丝体积分数为25%和3k碳纤维丝的C/CF先驱丝体积分数为44.7%的复合材料的抗拉强度达到较高值,分别为595MPa和587MPa,均为纯铜抗拉强度的3倍以上.3k丝制成的一次C/CF先驱丝内碳纤维丝的数量较多,影响复合材料的界面强度,而选用1k碳纤维丝比较有利.     

Influence of preparation temperature on the oxidation resistance and mechanical properties of C/SiC coated C/C composites

A C/SiC oxidation resistance coating was prepared on carbon/carbon (C/C) composites by slurry and pack cementation. The microstructure, oxidation resistance and mechanical properties of C/SiC coating prepared from 1773 to 2573 K were investigated. With the increase of the preparation temperature, the oxidation resistance of C/SiC coating increases, however, the flexure strength decreases gradually. The preparation of C/SiC coating on C/C composites results in the fracture behavior of C/C composites changing from pseudo-plastic to brittle failure model. The decrease of flexure strength is mainly attributed to the decrease of C/C matrix’ flexure strength at high temperature.     

Numerical simulation on thermal expansion coefficient of 3D braided C/C composites简

To effectively get the thermal expansion coefficient(CTE) of three-dimensional(3D) braided C/C composites and study the variations, a VC?? program with graphical user interfaces was obtained, based on the yarn unit model and numerical analysis. With the limited basic properties of carbon fibers and carbon matrix, CTE of 3D braided C/C composites is obtained at 85 °C. The deviation between the simulated and experimental axial CTE of 3D braided C/C composites is no more than 11 %. The effects of different parameters(including the braiding angle of 3D braided preform, the fiber volume fraction and the porosity of 3D braided C/C composites, and the elastic modulus, Poisson's ratio and CTEs of carbon fibers and carbon matrix) were analyzed with the program. The results show that the axial CTE of C/C composites decreases with the increase of the braiding angle, the fiber volume fraction, and the porosity of 3D braided C/C composites. The transverse elastic modulus of carbon fibers has the greatest effect on the axial CTE among the studied mechanical parameters, followed by the elastic modulus and Poisson's ratio of carbon matrix.     

Oxidation behavior of C/C composites with the fibre/matrix interface modified by carbon nanotubes grown in situ at low temperature

Carbon nanotubes (CNTs) were grown in situ on the fibre surface of unidirectional carbon fibre preform. The carbon fibre preform with nanotube modified fibres was then densified by chemical vapor infiltration to obtain CNT-reinforced C/C (CNT-C/C) composite. The effects of CNTs on the oxidation kinetics and mechanism of C/C composites were investigated. The results show that due to the growth of CNTs, a more perfect structure of pyrolytic carbon (PyC) and better fibre/PyC interface had been obtained, which in turn result in slower mass loss. Furthermore, higher graphitization degree leads to larger activation energy of CNT-C/C composite, compared with C/C composite.     

浸渍-碳化工艺对碳/碳复合材料力学性能的影响

采用碳纤维针刺整体毡作为增强体,硼酚醛树脂作为基体先驱体,用浸渍碳化的方法制备C/C复合材料.考察了在不同的浸渍压力和碳化温度下材料力学性能的差异.分析结果表明:不仅密度是影响碳/碳复合材料力学性能的重要因素,纤维和基体的结合状况以及基体碳的结构也是决定材料强度和断裂方式的重要因素.随着工艺参数的改变,碳/碳复合材料的断裂模式可以由“假塑性断裂”向“脆性断裂”转变.     

准三维C/C复合材料的层间剪切性能及其断裂机理

以炭纤维针刺毡为预制体, 采用化学气相浸渗(CVI)法或结合液相法制备了热解炭、树脂炭和沥青炭基质的准三维C/C复合材料, 研究了这些材料的层间剪切性能及其断裂机理. 结果表明: CVI基质炭比沥青基质炭更有利于C/C复合材料的层间剪切性能的提高; 剪切强度随密度增高而增大, 致密度越高, 基体支撑越强, 同时微裂纹和孔隙度就越低, 断裂裂纹不易形成或扩展, 强度性能就越好; 纯沥青基质炭试样为"突发"的脆性断裂方式, 其他基质炭试样表现为韧性断裂方式.     

Rapid chemical vapor infiltration of C/C composites

With liquid petrol gas (LPG) as carbon source, carbon felt as porous perform and hydrogen as diluent, C/C composites were fast fabricated by using a multi-physics field chemical vapor infiltration (MFCVI) process in a self-made furnace. A set of orthogonal experiments were carried out to optimize parameters in terms of indices of density and graphitization degree. The results show the optimal indices can be achieved under the conditions of temperature 650 °C, LPG concentration 80%, gas flux 60 mL/s, total pressure 20 kPa, infiltration time 15 h. The verification experiment proves the effectiveness of the orthogonal experiments. Under the optimal conditions, the graphitization degree of 75% and bulk density of 1.69 g/cm are achieved with a uniform density distribution. At the same time, a new structure is obtained.     

Effect of stress level on fatigue behavior of 2D C/C composites

Laminated carbon fiber clothes were infiltrated to prepare carbon fiber reinforced pyrolytic carbon (C/C) using isothermal chemical vapor infiltration (CVI). The bending fatigue behavior of the infiltrated C/C composites was tested under two different stress levels. The residual strength and modulus of all fatigued samples were tested to investigate the effect of maximum stress level on fatigue behavior of C/C composites. The microstructure and damage mechanism were also investigated. The results showed that the residual strength and modulus of fatigued samples were improved. High stress level is more effective to increase the modulus. And for the increase of flexural strength, high stress level is more effective only in low cycles. The fatigue loading weakens the bonding between the matrix and fiber, and then affects the damage propagation pathway, and increases the energy consumption. So the properties of C/C composites are improved.     

工艺因素对水热改性C/C复合材料抗氧化性能的影响

以一定配比的Al_2O_3粉和磷酸溶液组成的悬浮液作为水热处理前驱体,采用水热法对C/C复合材料基体进行了防氧化改性.采用X射线衍射(XRD)仪、扫描电子显微镜(SEM)和能量色散谱(EDS)仪分别对改性试样的物相组成、显微结构及化学元素组成进行表征.重点研究了水热反应时间、水热反应釜填充比等工艺因素对改性C/C复合材料的物相组成、微观形貌及抗氧化性能的影响.结果表明:水热改性方法是一种行之有效的提高C/C复合材料基体抗氧化性能的手段.经过水热改性处理,试样的抗氧化性能明显提高;延长水热反应时间和增大水热釜填充比都有利于基体抗氧化性能的提高;在水热釜填充比为70%、水热温度为200 ℃的条件下,改性处理72 h的C/C复合材料在700 ℃的静态空气中恒温氧化10 h后氧化失重仅为2.31%.     

中间相沥青基炭/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.     

表面硅化对C/C复合材料组织结构的影响

采用表面固相渗硅工艺在C/C复合材料表面制备SiC涂层 ,研究了制备工艺对涂层和C/C复合材料组织结构的影响。结果表明 :硅化反应时间对C/C复合材料的SiC涂层厚度影响不大 ;C/C复合材料组织中热解碳基体与碳纤维相比 ,更易与Si反应生成SiC ,说明碳纤维的稳定性高于热解碳 ,Si通过界面和材料缺陷扩散深入基体内部。     

炭/炭复合材料声电沉积钙磷生物活性涂层的生长机理

通过声电沉积在炭/炭复合材料表面制备钙磷生物活性涂层,采用SEM（带EDAX）,XDR,FTIR研究电沉积时间对钙磷生物活性涂层的形貌、结构和组成的影响.实验结果表明：沉积初始先在炭/炭表面形成无定形层,片状磷酸氢钙（DCPD）在其表面生长,随着电沉积时间的延长,逐渐向针状的羟基磷灰石Ca10（PO4）6（OH）2（HA）转变,涂层厚度和n（Ca）/n（P）不断增加,涂层的结晶度和电解液的pH值下降.涂层为缺钙磷灰石.同时探讨了在炭/炭复合材料表面钙磷生物活性涂层的生长机理.     

添加BN对光滑层热解炭结构的C/C复合材料摩擦性能的影响

通过粉末层铺法向全网胎炭纤维预制体中添加六方氮化硼粉末和化学气相沉积热解炭增密制备C/C-BN复合材料。在MM 1000摩擦试验机上对其摩擦磨损性能进行测试,并对摩擦表面进行光学形貌观察以及对材料的组织结构和磨屑进行SEM形貌观察。结果表明:与C/C复合材料相比,C/C-BN复合材料的线性磨损率降低了40%,质量磨损率降低了70%;摩擦表面中的六方BN在摩擦过程中始终保持稳定,BN的存在使光滑层热解炭结构的C/C复合材料的摩擦因数曲线变得平稳、波动小并且对刹车压力响应迅速,摩擦表面上形成了一层薄的摩擦膜。     

TENSILE TESTING OF C/C COMPOSITES ATHIGH TEMPERATURES

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高密度预制体制备炭/炭复合材料的弯曲力学性能与断裂机制

以丙烯作为碳源,氮气作为载气,采用初始密度为0.94g/cm3三维正交PAN基12K炭纤维预制体,利用自制的快速CVI炉制备基体热解炭结构为带状结构的C/C复合材料。力学性能测试结果表明,材料的弯曲断裂特征与制备过程中受到的高温热处理次数有关。从载荷-位移曲线来看,当C/C复合材料经过两次热处理时,C/C复合材料呈明显假塑性断裂特征。当C/C复合材料经过三次热处理时,载荷-位移曲线趋于稳定平滑,抗弯强度降低。从C/C复合材料断面的SEM图可以观察到材料断裂可以分为层间断裂和层内断裂,而层内断裂又因热解炭填充密度变化呈明显的分区断裂。由于热解炭和纤维含量在C/C复合材料中分布的差异,材料在不同的区域表现出不同的断裂特征,从而使得材料具备良好的弯曲强度同时具有一定的韧性特征。     

混杂C／C复合材料的烧蚀性能

利用等离子体火炬为高温热源，研究了混杂C／C复合材料的烧蚀性能。结果表明：随着烧蚀区域从火焰中心到边缘的变化，材料的烧蚀特性从中心区域的以热力学烧蚀为主向靠近边缘区域的以热化学烧蚀为主过渡；碳基体和碳纤维的抗热力学烧蚀性能相当，而碳纤维的抗热化学烧蚀特性则明显优于碳基体。