定向碳纳米管/炭纳米复合材料形貌和显微结构

以CVD法定向碳纳米管(ACNTs)阵列为骨架,利用化学气相渗透(CVI)工艺制备了新型定向碳纳米管/炭(ACNT/C)纳米复合材料。通过偏光金相显微镜(PLM)、扫描电子显微镜(SEM)、高分辨透射电子显微镜(HRTEM)、X射线衍射(XRD)和Raman光谱等分析方法对其显微结构和热解炭沉积机理进行了研究。结果表明:所制ACNT/C纳米复合材料的热解炭结构主要为类粗糙层结构,围绕碳纳米管生长的热解炭石墨层片结构清晰,并且碳纳米管和热解炭之间具有良好的界面结合;而在相同工艺条件下围绕炭纤维生长的热解炭为典型的光滑层结构。这可能是由于在热解炭沉积过程中存在碳纳米管"诱导"沉积过程,即沿着碳纳米管径向的离域化共轭π键和具有类似结构的芳香族大分子通过π-π非共价键作用相结合,并在CNTs纳米尺寸的影响下,芳香族大分子按照"软取向"(Softepitaxy)围绕碳纳米管生成环形层片状类石墨结构的热解炭。该研究结果有望为热解炭的可控沉积起到一定的借鉴作用。     

三维针刺碳毡增强碳/氮化硼复合材料的力学和介电性能

三维针刺碳毡中碳纤维的排布方式有利于电磁波的吸收。采用碳基体和氮化硼（BN）基体与三维针刺碳毡复合, 可望获得耐高温吸波复合材料。本文中采用先驱体浸渗裂解法（PIP）制备多孔三维针刺碳/碳（C/C）复合材料, 再利用化学气相渗透法（CVI）将BN引入C/C复合材料中, 最终获得了C/C--BN复合材料。研究了CVI时间对三维针刺C/C--BN复合材料微结构、 力学性能及介电性能的影响规律。随着CVI时间的增加, C/C--BN的密度增加, 孔隙率降低, 抗弯强度提高, 介电常数增加,介电损耗降低。在CVI时间达160h后, C/C--BN密度为1.43g/cm3, 总气孔率为25%, 抗弯强度达到82MPa。      

CVI-iC/TaC改性C/C复合材料的力学性能及其断裂行为

以针刺碳纤维整体毡为预制体,采用化学气相渗透工艺对预制体纤维进行PyC/SiC/TaC的多层复合模式的涂层改性, 然后采用化学气相渗透和热固性树脂浸渍-化进行增密,制备出新型C/C复合材料。对复合材料的微观结构和力学性能进行了研究。结果表明:包覆在碳纤维表面的PyC/SiC/TaC多层结构均匀致密、无裂纹,在C/C复合材料中形成空间管状网络结构;改性后C/C复合材料的抗弯强度和韧性均大大提高, 平均抗弯强度达到522 MPa,断裂位移达到1.19mm;复合材料弯曲断裂形式表现为脆性断裂,经过2000℃高温热处理以后,复合材料的抗弯强度下降,但最大断裂位移增大,弯曲断裂形式由脆性断裂转变为良好的假塑性断裂。      

Nicalon-fibre-reinforced silicon-carbide composites via polymer solution infiltration and chemical vapour infiltration

A new, faster process was developed for the fabrication of Nicalon-fibre-reinforced SiC composites by combining polymer solution infiltration (PSI) and chemical vapour infiltration (CVI). The process led to the near-net-shape fabrication of fibre-reinforced ceramic-matrix composites and reduced infiltration time. Typical flexural strength and fracture toughness of these composites were 296 MPa and 10.9 MPa m^1/2 at room temperature (RT) and 252 MPa and 9.6 MPa m^1/2 at 1000 °C, respectively. The composites exhibited load-carrying capability after crack initiation.     

电耦合CVI制备穿刺C/C喉衬材料的微结构及性能

采用电耦合化学气相渗透（CVI）联合树脂浸渍碳化工艺制备了穿刺碳纤维预制体增强C/C喉衬材料,利用μ-CT表征了穿刺C/C材料增密不同阶段孔隙尺寸,研究了该材料2 800℃拉伸性能和缩比固体发动机烧蚀性能。结果表明,电耦合CVI增密后穿刺C/C喉衬材料孔隙主要存在于纤维束间,呈现空间联通的网状结构,树脂碳循环致密后材料内部仍残存少量体积0~0.08 mm³的微小孔隙,孔隙呈现孤立的点分布状态。穿刺C/C材料2 800℃拉伸强度略高于室温,断裂应变比室温提高118%,表现出优异的非线性断裂行为。穿刺C/C喉衬缩比固体发动机点火试验后线烧蚀率0.077 mm/s,喉衬不同区域的烧蚀机制有一定差异,喉衬收敛段穿刺纤维束承受驻点烧蚀,产生蜂窝状烧蚀凹坑,烧蚀较严重,喉部和扩散段烧蚀较为平滑。     

Effect of multilayer coating on mechanical properties of Nicalon-fibre-reinforced silicon carbide composites

Nicalon-fibre-reinforced SiC composites were fabricated by combining polymer solution infiltration (PSI) and chemical vapour infiltration (CVI). Effect of multilayer coating on mechanical properties of the composites was investigated. The coatings consisted of chemically vapour deposited (CVD) C and SiC and were designed to enhance fibre pull-out in the composites. It was found that the flexural strength and fracture toughness of the composites were increased with the number of coating layers and was a maximum for 7 coating layers which consisted of C/SiC/C/SiC/C/SiC/C. Typical flexural strength and fracture toughness of the composites were 300 MPa and 14.5 MPa m^1/2, respectively.     

碳纤维上原位生长碳纳米管对C/C复合材料弯曲性能的影响

以碳毡为基底原位生长了碳纳米管（CNTs）,借助化学气相渗透制备了CNTs-C/C复合材料。研究了催化剂含量对碳纳米管生长的影响以及不同含量碳纳米管对C/C复合材料弯曲性能的影响。结果表明：催化剂对CNTs产量影响较大,且含量越多,生成的CNTs量越大;原位生长CNTs引入的催化剂会导致CNTs-C/C复合材料弯曲性能变差;CNTs的加入改变了热解碳的沉积行为,诱导了球状和锥状小尺寸热解碳的形成,减少了微裂纹的出现。适量CNTs能提高C/C复合材料的弯曲强度和模量,并改善材料的断裂行为。     

Static friction properties of carbon/carbon composites

Preforms were made from 1K PAN plain carbon cloth and densified using the rapid directional diffusion chemical vapor infiltration (RDD CVI) processes. Four carbon/carbon (C/C) composite specimens treated at 1800 (specimen A), 1800+2000 (B), 2000 (C), and 2300 °C (D), respectively, were prepared, then machined into ring-on-ring specimen configurations. The influence of high-temperature heat treatment and the test temperatures on the static friction properties of the C/C composites has been researched. The results show that the high-temperature heat treatment processes has an important impact on the static friction behaviors of RDD CVI C/C composites. With raising the treatment temperature, the interlayer spacing of the matrix carbon in them becomes small, and the crystallite width as well as height increase. Under the test at room temperature, the static friction coefficients (FC) of the specimen treated at 1800 °C (A) are the lowest, but become very big and the highest under the test temperature of 260 °C due to desorption of the water absorbed on the friction surface. The composites treated at 2000 °C (C) exhibit enough high static friction coefficients under room temperature owing to their absorption of less water and the difficult delamination of the matrix carbon. However, in the test temperature of 260 °C or after the dynamic friction tests, their static FC is low. The specimen treated at 2300 °C (D) has a low FC at 260 °C heat condition, but its FC is higher than that of A and C under room temperature and largest after dynamic friction tests. No matter how high the heated temperatures are, the static FC of C/C composites decreases with an increase of the brake-specific pressure. When the specific pressure is very high and exceeds a certain value, the static FC is almost the same for specimens B, C, and D.     

Preparation and properties of 2D C/ZrB2-SiC ultra high temperature ceramic composites

Two-dimensional C/ZrB₂-SiC composites were fabricated by chemical vapor infiltration (CVI) process combined with slurry paste (SP) method. ZrB₂ was introduced in the matrix by stacking the pasted carbon cloth with ZrB₂-polycarbosilane slurry. After heat-treated at 900 °C, the stacked carbon cloth preform was infiltrated SiC by CVI process to obtain 2D C/ZrB₂-SiC composites. Mechanical properties such as flexural strength and interlaminar shear strength were investigated. The ablation tests were carried out on an oxyacetylene torch flame. The small linear erosion rates indicate that the composites have good ablation resistance properties. These results demonstrate that CVI combined with SP method is a useful way to fabricate 2D C/ZrB₂-SiC composites.     

Effect of isotropic interlayers on the mechanical and thermal properties of carbon/carbon composites

Multilayer which consists of isotropic (ISO) interlayer and rough laminar (RL) and single RL structure carbon/carbon (C/C) composites have been prepared by isothermal chemical vapor infiltration at 5 and 1 kPa. Mechanical and thermal properties of both composites have also been studied. Experimental results indicate that ISO interlayer between fiber and matrix plays an important role on fracture behavior and strength of the composites. Comparing with single RL structure composites, the strength decrease of composites with ISO interlayers is about 28-40%. ISO interlayer is the main source of fracture due to its low density and micropores between crystallites. The low thermal conductivity of ISO interlayers also results in the thermal property degradation of obtained C/C composites. By reducing infiltration pressure, the ISO interlayers are substituted by compact RL matrix which improves the general properties of C/C composites.     

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.     

Reinforcement and antioxidizing of porous carbon by pulse CVI of SiC

In order to reinforce and antioxidize porous carbon, chemical vapour infiltration (CVI) of SiC was investigated using a repetitive cycle of evacuation of vessel and instantaneous source-gas filling. From a source gas of 5% CH₃SiCl₃-H₂, a temperature range of 1273 to 1373 K was considered to be suitable to infiltrate SiC into a deep level, and surface deposition was enhanced at above 1373 K which led to pore blockage. With 3000 pulses, flexural strength was improved from 35 to about 90 MPa. Several specimens were exposed to air at 1573 K for 1070h during which the specimens were cooled to room temperature between four and seven times. SiC felt was also obtained by oxidation of a carbon skelton after pulse CVI.     

基于遗传算法和神经网络的C/C复合材料等温CVI工艺参数优化模型

建立了基于遗传算法和误差反传（GA-BP）神经网络的化学气相渗透（CVI）工艺参数优化模型。以新型等温CVI工艺制备C/C复合材料时采集的实验数据作为模型评价样本,分析了主要可控影响因素（沉积温度、前驱气体分压与滞留时间等）对C/C复合材料制件密度及其密度均匀性的作用规律。在该模型指导下,样本的期望密度和实测密度最大误差不超过6.2%,密度差最大误差不超过8.2%。实验结果也证明了该模型具有较高的精度和良好的泛化能力,可以用于CVI工艺参数的优化。      

热处理对含CSiCTaCC界面C/C复合材料力学性能的影响

以准三维针刺炭纤维毡为预制体, 采用化学气相渗透工艺在预制体中炭纤维/基体炭之间制备C-SiC-TaC-C复合界面, 利用树脂浸渍-炭化工艺对材料进一步增密, 获得含C-SiC-TaC-C界面的C/C复合材料。研究了1400～2500℃不同温度热处理前后复合材料的微观结构和力学性能。结果表明: 热处理前, SiC-TaC界面为管状结构, 复合材料的抗弯强度为241.6 MPa, 以脆性断裂为主; 经1400～1800℃热处理后, TaC界面破坏呈颗粒状, 复合材料的平均抗弯强度下降到238.9～226.1 MPa, 其断裂方式不变, 但断裂位移由0.7 mm增至1.0 mm; 经2000～2500℃热处理后, SiC、 TaC界面均受到破坏, 复合材料平均抗弯强度急剧下降至158.7～131.8 MPa, 断裂方式由脆性断裂转变为假塑性断裂。      

温度脉冲方法制备碳/碳化硅复合材料界面的微观结构与性能研究

采用温度脉冲化学气相渗透沉积的方法制备了碳/碳化硅复合材料界面. 以六甲基二硅胺烷(Hexamethyldisilazane , HMDS) 为前驱体, 以3k, 三维四向的石墨化碳纤维编织体为预制体, 通过强制流动热力学梯度化学气相渗透沉积的方法(FCVI)制备出密度为1.98g·cm^-3的C _f/SiC复合材料. 运用透射电子显微镜(TEM)对复合材料的界面微观结构进行了分析. 复合材料的平均弯曲强度为458MPa, 平均断裂韧性为19.8MPa·m^1/2. 应用扫描电子显微镜(SEM)对复合材料的断裂形貌进行了分析研究.     

致密化工艺对厚壁针刺C/C复合材料性能的影响

采用化学气相渗透(CVI)+树脂浸渍碳化法(PIC)、CVI+沥青高压浸渍碳化法(HPIC)及HPIC工艺分别制备了IR-C/C、IP-C/C以及P-C/C三种厚壁针刺C/C复合材料,研究了三种材料的热力学性能及材料内部密度均匀性。结果表明,IP-C/C材料轴向拉伸强度为24.7 MPa,IR-C/C材料轴向压缩强度达到200 MPa,而P-C/C材料轴向拉伸强度仅为7.4 MPa,相比IR-C/C材料降低了53%,相比IP-C/C材料降低了70%。复合致密化工艺制备的材料具有较低的热膨胀系数,而P-C/C材料1000℃热膨胀系数达到了3.566×10-6℃-1,是IPC/C材料的2.5倍。IP-C/C材料和P-C/C材料采用高压碳化工艺增密,材料的致密度高,密度分布均匀,导热系数高。IR-C/C材料内部密度降为14.5%,密度分布为外高内低。以CVI+HPIC复合制备的材料综合性能优异,且内部密度分布均匀,适合于制备厚壁材料。     

含炔基酚醛树脂改性PSA及碳纤维布/PSA-EPAN复合材料性能

合成了乙炔基苯基偶氮酚醛树脂（EPAN）,通过溶液共混的方法用其对含硅芳炔树脂（PSA）进行改性,研究了PSA-EPAN树脂的热性能,并制备了PSA-EPAN的碳布预浸料,经热模压制备碳纤维布（T300CF）增强PSA-EPAN复合材料,对其力学性能进行了研究。结果表明：EPAN均匀分布于PSA树脂中,EPAN共混改性PSA树脂的固化温度提高,混入质量分数为7%的EPAN,N₂中固化PSA-EPAN树脂在800℃残留率超过90%,其玻璃化转变温度高于500℃,PSA-EPAN共混树脂浇铸体的弯曲性能高于PSA树脂,达40.7 MPa,提高了95.5%;PSA树脂经T300CF/PSA-EPAN复合材料力学性能显著提高,弯曲强度达到了423.5 MPa,提高了74%,层间剪切强度（ILSS）提高至29.53 MPa,增加了65%。     

Preparation and microstructural evolution of carbon/carbon composites

Carbon/carbon (C/C) composites with characteristic matrix-crack pattern are key intermediate materials for preparation of carbon/silicon carbide (C/C–SiC) composites. The C/C composites were prepared by pyrolyzing carbon fiber/phenolic resin preform. The change of density, open porosity, mass loss and specially the microstructural evolution of the composites during pyrolysis at 200–900 °C was analyzed, which provided important information for preparation of C/SiC composites by infiltration of silicon. An increasing number of regular spacing cracks were formed above 400 °C. After pyrolysis at 900 °C, the pore volume was 0.17 cm³/g, and the pores in the radius range of 2.44–122.19 μm occupied 81% of the pore volume.     

粘结MoS2基钼固体润滑膜的抗承载能力和耐速度性能研究EI

为了探讨粘结MoS2基固体润滑膜在干摩擦条件下的抗承载能力和耐速度性能,使用国产的环一块摩擦磨损试验机在干摩擦下对粘结MoS2基固体润滑膜在不同载荷和不同速度试验条件下的摩擦磨损性能进行了研究.试验结果表明:粘结MoS2基固体润滑膜的承载能力有高达2100N,在0.512～3.84m/s的滑动速度范围内具有良好的抗磨减摩性能.对转移膜的研究结果表明高载高速试验条件有利于促进对偶表面生成高质量的转移膜.粘结MoS2基固体润滑膜具有良好的抗承载能力和耐速度性能的机理应归结于在摩擦过程中对偶表面高质量转移膜的生成.     

Preparation of carbon microparticle assemblies from phenolic resin using an inverse opal templating method

Three-dimensionally (3D) well-ordered carbon microparticle assemblies with different particle morphologies were fabricated by infiltration of phenolic resin solution into SiO₂ inverse opal structures and subsequent carbonization. The effect of the phenolic resin solution concentration and the carbonization temperature on the morphology of the fabricated carbon microparticles was investigated. At a carbonization temperature of 1000 °C, carbon microparticles with interlocked bridges were obtained when the concentration of phenolic resin solution is 40 wt% and hollow carbon microparticles with opened window channels were obtained at a concentration of 30–35 wt%. When the carbonization temperature was decreased to 500 °C, carbon microparticles with interlocked bridges also were observed, even when the phenolic resin concentration was 30 wt%. The structures and properties of the carbon microparticles and their assemblies were characterized using SEM, XRD, and N₂ adsorption.