纤维种类对炭/炭复合材料微观结构和力学性能的影响(英文)

采用6 K的预氧丝和炭纤维制备预制体,通过化学气相渗积制备炭/炭复合材料。通过偏光显微镜、拉曼光谱、纳米硬度和三点弯曲等手段研究其微观结构和力学性能。结果表明,预氧丝复合材料的基体为暗层和粗糙层炭,厚度分别为1.4-2.6μm和10.2-11.6μm;而炭纤维复合材料的基体为光滑层和粗糙层炭,厚度分别为8μm和4.4μm;预氧丝纤维的模量和硬度明显小于炭纤维,同时基体的模量和硬度随消光角的增加而降低;低模量的基体和纤维导致预氧丝复合材料的拉伸强度、拉伸模量、弯曲强度和模量分别降低了14.5%-24.2%、9.7%-19.8%、7.3%-15.4%和15.1%-18.6%;但其韧性指数却提高了224%-235%,这是高含量的粗糙层炭和纤维的石墨化收缩所致;同时提出了一个三单元复合模型用来模拟复合材料的拉伸模量,模拟误差小于9.9%。     

炭泡沫的制备、性能及应用

炭泡沫是具有广阔应用前景的新型炭材料,自出现起就成为炭材料研究中的热点.以中间相沥青基炭泡沫为重点,介绍了炭泡沫的发展历史和研究进展,总结了现有炭泡沫制备技术,包括发泡剂发泡法、模板法、中间相沥青自发泡法和限空间法等,概述了炭泡沫的性能和应用前景,并展望了其发展方向.     

沥青炭的微观结构对其压缩强度的影响

将高温煤沥青和浸渍剂沥青在不同压力下炭化,在2500℃下对所得沥青炭进行石墨化处理;测试了所得沥青炭的体积密度、开孔率;利用扫描电子显微镜（SEU）观察了所得沥青炭的显微结构;利用XRD检测了所得沥青炭石墨化处理后的石墨化度;测试了所得沥青炭的压缩强度。结果表明：随着炭化压力的增大,沥青炭的体积密度增大而开孔率减小,压缩强度也随之增大;随着炭化压力的增大沥青炭显微结构呈由流线型向镶嵌型和域型转变的趋势;流线型结构沥青炭石墨化度较高,但也导致沥青炭的压缩强度降低。     

纤维含量和热处理对炭/炭复合材料性能的影响

研究了炭纤维体积分数和预制体热处理温度对炭/炭复合材料力学性能的影响.结果表明,随着预制体中炭纤维体积分数的增加炭/炭复合材料的硬度逐渐增加,但当炭纤维的体积分数大于30%时,炭/炭复合材料硬度增加的幅度减小.炭纤维体积分数的增加对炭/炭复合材料硬度的影响有两个相反的作用,纤维的增强作用将使硬度增大,而孔隙率的增加将导致硬度的减小.炭/炭复合材料的抗弯强度随着纤维体积分数的增加而增加,但因纤维体积分数的增加会导致孔隙减小.致使热解炭不能充分地渗透填充到纤维间的孔隙内,抗弯强度下降,所以随着纤维体积分数的增加,材料的弯曲强度会出现拐点.随着预制体热处理温度的不同,炭/炭复合材料有脆性断裂、整束纤维拔出的假塑性断裂和部分炭纤维拔出的假塑性断裂三种断裂机制.     

沥青基炭纤维γ-射线改性对炭/ 炭复合材料力学性能的影响

为了提高沥青基炭纤维表面活性, 采用γ-射线辐照对沥青基炭纤维表面改性。用AFM、XPS 研究了γ-射线辐照改性后沥青基炭纤维表面结构的变化, 用浸润仪测定了改性前后沥青基炭纤维表面能的变化。研究了γ-射线辐照沥青基炭纤维对炭/ 炭复合材料力学性能的影响, 并用SEM 分析了炭/ 炭复合材料断口形貌。结果表明,γ-射线辐照使炭纤维表面含氧官能团和表面粗糙度增加, 提高了沥青基炭纤维的表面能; 降低了炭/ 炭复合材料孔隙率, 提高了炭/ 炭复合材料力学性能。     

热处理温度对热解炭及炭/炭复合材料力学性能的影响

以丙烷为气源,采用等温等压化学气相渗透技术制备了炭/炭复合材料,利用X射线衍射、偏光显微镜、扫描电镜、纳米压痕仪、三点弯曲法研究了热处理温度对热解炭以及炭/炭复合材料微观结构和力学性能的影响.微观结构观察显示随着热处理温度的升高,热解炭层间距减小,同时石墨化度提高;由于发生了局部应力石墨化,热解炭出现同心微裂纹,并且随热处理温度的升高裂纹的数量和宽度增加.纳米压痕测试表明,热解炭的纳米压痕行为是完全的弹性形变,完全卸载后热解炭表面没有残余压痕,但加载和卸载曲线没有重合而是存在一定的能量耗散,随着热处理温度的升高,热解炭的弹性模量增大.热处理后纤维强度降低,并且纤维与基体炭界面脱离,导致炭/炭复合材料的弯曲强度和模量下降.     

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.     

热解炭过渡层-中间相沥青基炭/炭复合材料的微观结构

借助偏光显微镜、扫描电镜、透射电镜对具有热解炭过渡层的中间相沥青基炭/炭复合材料的微观结构进行了研究。结果表明:材料的基体由热解炭和中间相沥青炭组成,在偏光显微镜下均呈现出光学各向异性。材料内部形成了多层次的界面结构,热解炭与纤维的界面连续,界面层内的石墨微晶择优取向度较高,晶格条纹排列规整;中间相沥青炭与热解炭界面不连续,为"裂纹型"界面,界面层内主要为非晶态碳。材料中炭纤维、热解炭、中间相沥青炭的石墨微晶大小逐渐增大,择优取向度逐渐增高,晶格条纹的排列逐渐规整。片层条带状结构的中间相沥青炭以及材料内的微裂纹平行于炭纤维轴向。     

炭/炭复合材料用基体前驱体煤沥青的研究动态

综述了近年来炭／炭复合材料用基体前驱体煤沥青的研究动态，重点阐述了不同改性方法对煤沥青的残炭率及高温流变性能的影响，指出了开发综合性能优良的改性煤沥青是制备低成本高性能炭／炭复合材料的关键。     

中间相沥青的应用研究进展

中间相沥青是制备多种高级炭材料的优质原料,在高新材料领域引起了广泛关注.介绍了中间相沥青的基本性质以及国内外以中间相沥青为原料制备沥青基炭纤维、泡沫炭、多孔炭、电极材料等新型炭材料的研究现状,展望了中间相沥青的应用前景.     

The effects of plasma pre-treatment and post-treatment on diamond-like carbon films synthesized by RF plasma enhanced chemical vapor deposition

Diamond-like carbon (DLC) films were synthesized by RF plasma enhanced chemical vapor deposition and the effects of plasma pre-treatment and post-treatment on the DLC films were investigated. Experimental results show that the surface roughness of the substrate, ranging from 0.2 to 1.2 nm, created by the plasma pre-treatment, will affect the surface roughness of the DLC films deposited using methane as the carbon source. However, the film surface roughness (0.1-0.4 nm) is much smaller than that of the substrate. Raman analysis and hardness measurement by nanoindentation indicate that the structure and the hardness of the DLC films are relatively unchanged for the film surface roughness investigated. For the argon or hydrogen plasma post-treatment of the DLC films deposited using acetylene as the carbon source, it is found that surface roughness decreases with the post-treatment time. Although the hardness decreases after post-treatment, it remains relatively constant with increasing post-treatment time.     

Surface characterization and nanomechanical properties of diamond-like carbon films synthesized by RF plasma enhanced chemical vapor deposition

Diamond-like carbon (DLC) films were synthesized by RF plasma enhanced chemical vapor deposition using acetylene as the carbon source and the effects of acetylene/nitrogen ratio in the reaction atmosphere, deposition pressure, and plasma post-treatment using different atmospheres on the surface roughness and mechanical properties of DLC films were investigated. Although the surface roughness, characterized by AFM, decreased as the acetylene/nitrogen ratio in the reaction atmosphere decreased, the hardness of DLC films measured by nanoindentation also decreased with the decrease of the acetylene/nitrogen ratio, which is consistent with the Raman results of the I_D/I_G ratio. Rougher films with higher residual stress were obtained when using a deposition pressure higher than 40.0 Pa (0.3 torr). For the effect of plasma post-treatment using different atmospheres, surface smoothing was found for the hydrogen plasma post-treatment, whereas nitrogen and argon plasma post-treatments resulted in surface roughening. Hydrogen plasma post-treatment was found to lower the surface roughness without significantly sacrificing the hardness.     

Mechanical characterization of fibres used for reinforcing metals and evaluation of seeded sol-gel derived alumina-fibre reinforced 1100 aluminium castings

The properties of a newly developed seeded sol-gel-derived alumina fibre have been evaluated and compared with currently commercially available alumina and pitch-derived carbon fibres of similar modulus. These fibres were wrapped into preforms and pressure infiltration cast to form commercially-pure-aluminium (1100) matrix composites. The manufactured composites were then flexure and tensile tested to determine their axial and transverse properties. Calculations of the composite strength based upon the statistical theory of fracture were performed and are in good agreement with the experimental results.     

Mechanical properties and thermal stability of nitrogen incorporated diamond-like carbon films

The nitrogen incorporated diamond-like carbon films were deposited on Si (100) substrates by arc ion plating (AIP) under different N₂ content in the gas mixture of Ar and N₂. The influence of N₂ content on the film microstructure and mechanical properties was studied by atomic force microscopy, transmission electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and nanoindentation. It was found that the hardness (H), elastic modulus (E), elastic recovery (R) and plastic resistance parameter (H/E) decrease with increasing the nitrogen content. The decrease of mechanical properties of DLC films resulted from nitrogen incorporation was associated with total sp³ carbon bond content and N-sp³C bond content. The structural modification as well as mechanical properties of the annealed nitrogen incorporated diamond-like carbon films was investigated as a function of annealing temperature. Raman spectra indicate that the I_D/I_G ratio starts to increase and G peak position shifts upward at the annealing temperature over 500 °C. The hardness and elastic modulus of thermally annealed nitrogen incorporated DLC films decreased slightly at lower annealing temperature and then significantly decreased at higher annealing temperature. The strong covalent bonding between C and N atoms is expected to be effective on their thermal stability enhancement.     

KOH活化法制备双电层电容器用高性能活性炭

以一种各向同性沥青为原料,通过不同恒温时间制备了具有不同软化点的两种中间相沥青,而后直接用KOH活化获得活性炭.考察了中间相沥青软化点对所得活性炭结构的影响,研究了以所制活性炭为电极材料的双电层电容器的性能.结果表明:两种中间相沥青的软化点分别为280℃和330℃,所得活性炭的比表面积分别为1337m2·g-1和1300m2·g-1.以两种活性炭为电极材料的双电层电容器在放电电流密度为50mA/g时的比容量分别为190.8F·g-1和255.6F·g-1.循环伏安测试表明:较低软化点中间相沥青制备的活性炭电极材料具有较好的矩形形状.     

Multi-Wall Carbon Nanotubes/Styrene Butadiene Rubber (SBR) Nanocomposite

A floating catalyst chemical vapor deposition (FC-CVD) method was designed and fabricated to produce high-quality and -quantity carbon nanotubes. The design parameters like the hydrogen flow rate; reaction time and reaction temperature were optimized to produce high yield and purity of Multi-Wall Carbon Nanotubes (MWCNTs). Multi-Walled Carbon Nanotubes (MWNTs) were used to prepare natural rubber (NR) nanocomposites. Our first efforts to achieve nanostructures in MWNTs/styrene butadiene rubber (SBR) nanocomposites were formed by incorporating carbon nanotubes in a polymer solution and subsequently evaporating the solvent. Using this technique, nanotubes can be dispersed homogeneously in the NR matrix in an attempt to increase the mechanical properties of these nanocomposites. The properties of the nanocomposites such as tensile strength, tensile modulus, elongation at break and hardness were studied. Using different percentages of carbon nanotubes from 1 wt% to 10 wt%, several nanocomposites samples were fabricated. Significant improvements in the mechanical properties of the resulting nanocomposites showed almost 10% increase in the Young's modulus for 1 wt% of CNTs and up to around 200% increase for 10 wt% of CNTs.     

纺丝液合成因素对木材液化物炭纤维原丝性能的影响

利用木材苯酚液化物合成纺丝液, 熔融纺丝制成新的炭纤维原丝, 研究了纺丝液合成因素对原丝性能的影响。试验结果表明: 增加合成纺丝液时液化原料中的苯酚/木材比(液固比), 则原丝的力学性能提高明显, 其中液固比由3增加至4时, 原丝拉伸强度增加了近9倍; 合成剂用量的增加却导致原丝力学性能的降低, 当合成剂用量为6%时, 原丝的拉伸强度和拉伸模量降幅较明显, 而断裂伸长率的最大降幅却出现在合成剂用量为4%时; 原丝的拉伸强度和拉伸模量随合成温度的升高而增加, 但增幅较小, 断裂伸长率随合成温度的升高却呈下降趋势, 且从110℃升高到115℃时断裂伸长率降幅较大; 原丝的力学性能随合成纺丝液升温时间的增加而先升高后降低, 升温时间为40min时制备的炭纤维原丝的力学性能最优。      

炭化压力对石墨化沥青焦微观结构的影响

以高温煤沥青为原料,分别在30MPa和60MPa炭化压力下制备了石墨化沥青焦,研究了两种炭化压力下制备的石墨化沥青焦的微观结构.结果表明：30MPa所制备试样的流线/流域型组织占优,60MPa制备试样的流域型和镶嵌型组织占优.流线型和流域型结构是易石墨化结构,镶嵌型结构是难石墨化结构.炭化压力对沥青焦微观结构的影响主要是通过影响中间相的成核、生长和融并来实现的,30MPa炭化压力下,中间相小球融并完全,因而形成各向异性流线型结构;60MPa炭化压力下,中间相小球融并受阻,从而形成镶嵌型结构.TEM和SAED分析表明：30MPa制备的石墨化沥青焦以高度取向的流线型组织为主,在片层边缘及片层之间存在各向同性组织;60MPa制备的石墨化沥青焦为多种微观组织并存,分布不均匀,除各向同性组织外,沥青焦微观组织选区电子衍射图谱的（002）环不同程度呈点状分布.以上现象说明30MPa制备的石墨化沥青焦微观组织的均匀性和取向性都要好于60MPa制备的石墨化沥青焦.     

Combination of Instrumented Nanoindentation and Scanning Probe Microscopy for Adequate Mechanical Surface Testing

The elastic indentation modulus and hardness of standard bulk materials and advanced thin films were deter-mined by using the nanoindentation technique followed by the Oliver- Pharr post-treatment. After measure-ments with different loading/unloading schemes on chemically polished bulk titanium a substantial decrease of both modulus and hardness vs an increasing loading time was found, Then, hard nanostructured TiBN and TiCrBN thin films deposited by magnetron sputtering (using multiphase targets) on substrates of high roughness (sintered hard metal) and low roughness (silicon) were studied. Experimental modulus and hardness characterized by using two different nanoindenter tools were within the limits of standard deviation. However, a strong effect of roughness on the spread of the experimental values was observed and it was found that hard-ness and elastic indentation modulus obeyed a Gaussian distribution. The experimental data were discussed together with scanning probe microscopy (SPM) images of typical imprints taken after the nanoindentation tests and the local topography's strong correlation with the results of nanoindentation was described.     

C-Ti nanocomposite thin films: Structure, mechanical and electrical properties

Carbon-titanium nanocomposite thin films were deposited by DC magnetron sputtering on oxidized silicon substrates in argon. The films were prepared at different deposition temperatures between 25 and 800 °C. Transmission electron microscopy was used to determine the structure of the films. All the C-Ti nanocomposites consisted of columnar TiC structure with average column width ∼10 and 20 nm and a thin carbon matrix. The thickness of the carbon matrix between adjacent TiC columns was ∼2-5 nm.Mechanical properties (hardness, reduced modulus) of C-Ti films showed a distinct variation depending on the deposition temperature. Films deposited at 200 °C had the highest hardness ∼18 GPa and the highest reduced modulus ∼205 GPa.Temperature dependence of the film resistance was measured between 80 and 330 K. C-Ti nanocomposites have a non-metallic conduction mechanism characterized by a negative temperature coefficient of resistivity (TCR). The most negative TCR was observed for films showing high hardness and reduced modulus of elasticity.