以环己烷为前驱体制备炭/炭复合材料

以环己烷为前驱体利用化学液气相沉积工艺,采用针刺炭纤维毡为预制体,制备了具有光滑层和粗糙层结构的炭/炭复合材料。利用金相显微镜、高分辨扫描电子显微镜进行了材料的微观组织结构的分析,分析了在不同位置不同织构热解炭的形成机理。同时阐述了化学液气相沉积工艺原理。实验结果表明,通过调整工艺参数,利用化学液气相沉积工艺可以制备具有不同微观组织结构的炭/炭复合材料。     

针刺炭纤维预制体结构单元对C/C复合材料性能的影响

采用6K炭纤维无纬布/网胎交替叠层及12K炭纤维无纬布/网胎交替叠层,在针刺工艺,致密化、热处理工艺完全相同的情况下,制备了密度为1.8g/cm3的热解炭/树脂炭双元基体的两种C/C复合材料产品,考察了针刺预制体结构单元对C/C复合材料性能的影响.结果表明,两种C/C复合材料的热学（垂直方向导热系数）、电学性能及石墨化度基本相当;而针刺6K炭纤维无纬布/网胎预制体C/C复合材料的拉伸、弯曲、压缩、层间剪切强度分别为127MPa,189MPa,263MPa,24.6MPa;其平行方向导热系数为54.6W/m＆#183;K,比常规针刺12K炭纤维无纬布/网胎预制体C/C复合材料相应提高了38％,32.2％,32.8％,38.9％,21％,彰显了细化针刺预制体结构单元对C/C复合材料力学性能的显著影响.     

新型炭纤维/泡沫炭预制体的制备及致密化研究

由炭纤维/酚醛树脂经过发泡、固化和炭化制备出4种不同炭纤维含量(3%,7%,10%和15%)的泡沫炭作为制备炭/炭复合材料新型预制体,通过等温化学气相沉积对预制体进行致密化处理。研究了炭纤维含量对预制体微观结构、致密化过程及力学性能的影响。结果表明:炭纤维含量增加,使预制体产生更多的微裂纹,并有更多的炭纤维裸露在泡沫炭韧带外,有助于提高化学气相沉积的沉积速率。炭纤维/泡沫炭预制体炭/炭复合材料压缩强度随着预制体中炭纤维含量的增加而增加,当炭纤维体积分数为10%时,压缩强度达到峰值,为43MPa。     

基于液相热解沉积的C/C复合材料及其热物性研究

环己烷为前驱体,以体密度0.50g/cm~3左右的T700(12k)炭纤维针刺毡为预制体,在自主设计的专用设备中用化学液相热解沉积工艺再结合热等静压工艺制备出1.75 g/cm~3C/C复合材料。借助偏光显微镜、扫描电镜对C/C复合材料的微观结构进行了研究,用耐驰NETZSCH LFA 457 MicroFlash激光热导仪对C/C复合材料热物性进行了分析,结果表明,该液相热解沉积工艺制备的C/C复合材料炭相多为粗糙层结构,沉积炭呈环形紧密包覆在炭纤维周围,炭纤维力学性能得以充分发挥。热物理性能测试结果表明,该复合工艺制备的C/C复合材料导热性能良好,热力学性能呈明显各向异性,线膨胀系数小,体积稳定性好。     

不同预制体结构C/C复合材料的CVI致密化行为

采用化学气相渗透(CVI)工艺分别对整体毡和针刺毡厚壁预制体进行了500 h的致密化,研究了2种预制体的致密化效率、微观结构及密度分布情况。结果表明:预制体结构对C/C复合材料的致密化行为影响较大。致密化前期,整体毡预制体表现出较高的致密化效率,后期效率下降较快,热解炭包裹在纤维之间,材料内部密度分布不均,呈现两边高中间低的现象。针刺预制体在CVI前期致密化效率较低,热解炭主要包裹在纤维束外,致密化后期致密化效率下降较慢,致密后材料内部密度分布均匀。与整体毡预制体相比,针刺预制体的孔隙平直,分布均匀,更有利于碳源气体的深入渗透以获得均匀的密度分布。     

致密工艺对C/C复合材料摩擦性能的影响

采用针刺全炭纤维网胎无纬布整体结构预制体为骨架，经化学气相沉积（CVD）、树脂浸溃（RD固化致密及炭化、石墨化制得C／C复合材料。研究了粗糙层（RL）和树脂炭（RC）对摩擦性能的影响。结果表明，RL结构的C／C复合材料的摩擦性能较好，稳定性较高，是用作飞机刹车材料的前提；采用CVD＋RI制备且石墨化后的C／C复合材料具有优良的摩擦磨损特性；CVD试样的密度较低时，摩擦系数较高，但磨损较大，较难形成完整的摩擦膜。     

PyC/SiC界面改性C/C-SiC-ZrC复合材料的等离子烧蚀性能研究

以丙烯(C3H6),三氯甲基硅烷(MTS)为原料,利用化学气相渗透(CVI)技术在炭纤维预制体的纤维表面依次制备了热解炭(PyC)与碳化硅(SiC)界面层,随后结合CVI及前驱体浸渍裂解(PIP)工艺对材料进行增密,制得了密度为1.92 g/cm3的界面改性C/C-SiC-ZrC复合材料.利用X射线衍射仪(XRD)与扫...     

针刺炭纤维预制体的发展与应用

对比了国内外针刺炭纤维预制体的发展与应用.法国Sneema公司采用针刺技术成型的预制体有Novoltex和Naxeco两种,应用于火箭发动机延伸锥、喉衬等.国产薄壁针刺C/C复合材料性能与法国针刺扩张段材料性能相当.国产针刺预制体有整体毡和炭布/网胎针刺预制体,炭布/网胎叠层针刺预制体由于x-y向引入了连续纤维,制品整体性能较好.针刺技术是炭纤维预制体的自动化成型技术,拓宽了C/C复合材料应用领域.     

高性能C/C复合材料制备工艺研究

对制备C/C复合材料的化学气相渗透工艺进行了系统的实验研究,着重分析了热解碳的沉积过程。研究表明,在化学气相渗透的初始阶段,热解碳主要在碳纤维表面沉积,并与碳纤维之间形成了界面结合;随后,热解碳的沉积继续填充碳纤维预制体内部的气孔。这一过程有助于缓解纤维与陶瓷基体之间的界面应力。研究表明,通过调节热解碳的沉积时间可以得到具有一定密度梯度的C/C复合材料。     

载气条件对C/C复合材料CVI致密化效率及性能的影响研究

以天然气为碳源前驱体、N₂作为载气,采用等温、等压化学气相渗透(CVI)工艺,对初始密度为0.42g/cm³的预制体针刺毡进行致密得到C/C复合材料,本文研究了载气条件对C/C复合材料的致密化效率、微观结构及性能的影响。研究结果表明,沉积温度1050℃、沉积压力4KPa条件下,沉积120h后送N₂(天然气与N₂的比例为5∶1),300h致密化后C/C复合材料的密度可达到1.46g/cm³,表观和内层的密度差异仅为0.07g/cm³;复合材料表面可看到明显的预制体孔隙,未出现结壳情况;弯曲强度可达到107.8MPa,断口形貌以假塑性断裂为主,纤维与热解碳之间结合良好;在1000℃下垂直纤维方向的最大热膨胀系数仅为0.925×10^-6/℃,说明复合材料具有优异的热力学性能。     

Nanographite-reinforced carbon/carbon composites

Carbon/carbon composites (C/Cs) with nanographite platelets (NGP) filler in a matrix derived from phenolic resin were produced. Different weight concentration (0.5, 1.5, 3, 5 wt.%) NGP were introduced by spraying the NGP during the prepreg formation. The NGP-reinforced C/Cs were characterized for effect of NGP concentration on microstructure, porosity, interlaminar shear strength (ILSS), flexural, ultrasonic and vibration damping behavior. At 1.5 wt.% NGP C/C, the highest values of ILSS observed was 10.5 MPa (increased by 22%), flexure strength of 142.4 MPa (increased by 27%), flexural modulus of 59.2 GPa (increased by 68%) and porosity of 18.8% (reduced by 17.5%) in comparison to neat (without NGP) densified C/C. Ultrasonic testing revealed an average increase of 15% through the thickness Young’s modulus of NGP-C/C; (3.12 GPa at 1.5 wt.% NGP). A 20% average decrease in the damping ratio of the first four modes of vibration was observed in 1.5 wt.% NGP densified C/C. At low concentration (⩽1.5 wt.%) the NGP filled in the pores, cracks and debonded interface but at concentration higher than 1.5 wt.% NGP lost their effectiveness due to agglomeration. The required cycles for desired density/properties are projected to be less compared to neat C/C due to less porosity observed in ⩽1.5 wt.% NGP concentration C/C.     

Pulsed electrodeposition of carbon nanotubes-hydroxyapatite nanocomposites for carbon/carbon composites

Carbon nanotubes-hydroxyapatite (CNTs-HA) composite coatings, which behaved like single composites, were synthesized by a combined method composed of electrophoretic deposition and pulsed electrodeposition. The phase compositions and the microstructure of the composite coatings were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transform infrared spectrometry (FTIR). Potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) studies showed that the CNTs-HA composite coatings protected the bare carbon/carbon composites from corrosion in simulated body fluid (SBF) solution. The adhesion strength of CNTs-HA composite coating prepared by the combined method is 14.57±1.06 MPa achieved at the CNTs EPD time of 10 min. Compared to the other CNTs-HA composite coatings with different content of CNTs, the CNT-HA composite coating with the electrophoretic deposition of 10 min showed the best corrosion resistance. The morphology of CNTs-HA composite coatings immersed in SBF solution rendered the formation of HA crystallites. In addition, in vitro cellular responses to the CNTs-HA composite coatings were assessed to investigate the proliferation and morphology of mouse cells 3T3 cell line.     

Single-walled carbon nanotube buckypaper and mesophase pitch carbon/carbon composites

Carbon/carbon composites consisting of single-walled carbon nanotube (SWCNT) buckypaper (BP) and mesophase pitch resin have been produced through impregnation of BP with pitch using toluene as a solvent. Drying, stabilization and carbonization processes were performed sequentially, and repeated to increase the pitch content. Voids in the carbon/carbon composite samples decreased with increasing impregnation process cycles. Electrical conductivity and density of the composites increased with carbonization by two to three times that of pristine BP. These results indicate that discontinuity and intertube contact barriers of SWCNTs in the BP are partially overcome by the carbonization process of pitch. The temperature dependence of the Raman shift shows that mechanical strain is increased since carbonized pitch matrix surrounds the nanotubes.     

Kinetics of pyrolytic carbon infiltration for the preparation of ceramic/carbon and carbon/carbon composites

Carbon/carbon and zeolite/carbon composites have been prepared by pyrolytic carbon infiltration of organic and inorganic substrates with different porous structures. The chemical vapour infiltration kinetics of these substrates has been studied in a thermogravimetric system at atmospheric pressure, using benzene as pyrolytic carbon precursor. The rate of pyrolytic carbon infiltration seems to depend on the porosity of the substrate available to the pyrolytic carbon precursor, irrespective of the nature of the substrate studied. Activation energy values of about 180 kJ/mol were found for the different substrates used in the temperature range of 700-800 °C, where the cracking reaction of benzene takes place, predominantly, in a heterogeneous form. At higher temperatures homogeneous reactions compete with heterogeneous ones and higher values of activation energies (280-380 kJ/mol) were obtained. The oxidation of the pyrolytic carbon deposited on the different substrates studied takes place in the same range of temperature, which suggests the presence of a similar pyrolytic carbon structure on substrates of different nature or a similar accessibility to the deposited layer.     

Mechanical behavior of two-dimensional carbon/carbon composites with interfacial carbon layers

Effect of interfacial carbon layers on the mechanical properties and fracture behavior of two-dimensional carbon fiber fabrics reinforced carbon matrix composites were investigated. Phenolic resin reinforced with two-dimensional plain woven carbon fiber fabrics was used as starting materials for carbon/carbon composites and was prepared using vacuum bag hot pressing technique. In order to study the effect of interfacial bonding, a carbon layer was applied to the carbon fabrics in advance. The carbon layers were prepared using petroleum pitch with different concentrations as precursors. The experimental results indicate that the carbon/carbon composites with interfacial carbon layers possess higher fracture energy than that without carbon layers after carbonization at 1000°C. For a pitch concentration of 0.15 g/ml, the carbon/carbon composites have both higher flexural strength and fracture energy than composites without carbon layers. Both flexural strength and fracture energy increased for composites with and without carbon layers after graphitization. The amount of increase in fracture energy was more significant for composites with interfacial carbon layers. Results indicate that a suitable pitch concentration should be used in order to tailor the mechanical behavior of carbon/carbon composites with interfacial carbon layers.     

Friction behaviors of carbon/carbon composites with different pyrolytic carbon textures

Friction and wear properties of carbon/carbon (C/C) composites with a smooth laminar (SL), a medium textured rough laminar (RL) and a high textured RL pyrolytic carbon texture were investigated with a home-made laboratory scale dynamometer to simulate airplane normal landing (NL), over landing (OL) and rejected take-off (RTO) conditions. The morphology of worn surfaces at different braking levels was observed with scanning electron microscopy. The results show that C/C composites with RL have nearly constant friction coefficients, stable friction curves and proper wear loss at different braking levels, while friction coefficients of C/C composites with SL pyrolytic carbon decrease intensely and their oxidation losses increase greatly under OL and RTO conditions. Therefore, C/C composites with a high and medium textured RL pyrolytic carbon may satisfy the requirements of aircraft brakes. The good friction and wear properties of C/C composites with RL are due to the properties of RL, which leads to a uniform friction film forming on the friction surface.     

Microstructure of carbon/carbon composites reinforced with pitch-based ribbon-shape carbon fibers

Carbon/carbon composites were prepared with ribbon-shape pitch-based carbon fibers serving as reinforcement and thermosetting PFA resin and thermoplastic pitch as matrix precursors. The composites were heat treated to 1000, 1600 and 2700 °C. Microstructural transformations taking place in the reinforcement, carbon matrix, and the interface were studied using polarized optical and scanning electron microscopy. The fiber/matrix bond and ordering of the carbon matrix in heat-treated composites was found to vary depending on the heat treatment temperature of the fibers. Stabilized fiber cleaved during carbonization of resin-derived composites. In contrast, fibers retain their shape during carbonization of pitch matrix composites. Optical activity was observed in composites made with carbonized fibers; the extent decreases with increased heat treatment of the fibers. Studies at various heat treatment temperatures indicate that ribbon-shape fibers developed ordered structure at 1600 °C when co-carbonized with thermosetting resin or thermoplastic pitches.     

Sharp indentation behavior of carbon/carbon composites and varieties of carbon

Sharp indentation tests on carbon fiber and carbon matrix composites (C/C composite) were carried out over a wide load range from 0 to 2 N on three different cross sections: normal, parallel and inclined to the fiber axis. For comparison purposes, a variety of carbons including HOPG, glassy C, and pyrocarbon films was also examined. Both the fibers and the matrices displayed first a purely elastic response and second crack-induced damage. A purely elastic behavior was also observed with most of the varieties of carbon considered. Young’s modulus was extracted from the indentation curves either at maximum or at various forces, using the Sneddon equation of elastic response on loading (elastic indentation) or a classical equation based on elastic recovery on unloading (elastoplastic indentation). Results are discussed with respect to features of structure and heterogeneity of material in the stressed volume.