原位生长纳米纤维改性C/C复合材料的微观结构及性能研究
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摘要
本研究采用催化化学气相法(CCVD)在预制体内炭纤维表面原位生长纳米炭纤维(CNF)或纳米碳化硅纤维(SiCNF),随后采用化学气相渗透法(CVI)增密热解炭,制备了纳米纤维改性C/C复合材料,系统地研究了原位生长纳米纤维改性C/C复合材料(NF-C/C)的微观结构及导热、力学、氧化和摩擦磨损性能,并对比研究了CNF和SiCNF两种不同结构的纳米纤维改性对C/C复合材料的结构和性能的影响机理。主要研究内容和结果如下：
1.原位生长纳米纤维影响了炭纤维皮层结构的变化。在制备催化剂时,镍颗粒通过扩散进入炭纤维皮层,导致周围的碳原子重新排列,形成大微晶尺寸的高度有序石墨层,提高了炭纤维的石墨化度。在CCVD过程中,镍颗粒通过碳原子或碳化硅的内扩散从炭纤维皮层脱出。碳原子进入炭纤维皮层后修复炭纤维皮层的结构,并逐渐沉积在炭纤维表面形成中织构热解炭(MT-PyC)；碳化硅进入炭纤维皮层后,导致周围碳原子更加有序地排列。
2.纳米纤维诱导形成高织构热解炭(HT-PyC),并导致炭纤维与炭基体之间形成了一层界面层。包覆在CNF表面的PyC以HT-PyC的形式存在,并且在炭纤维与基体之间形成一层依次由MT-PyC、 CNF+HT-PyC组成的界面层；而包覆在SiCNF表面的PyC以MT-PyC和HT-PvC两种形式存在,MT-PyC介于SiCNF和HT-PvC之间,并在炭纤维与基体之间形成了一层由MTYUPvC、SiCNF以及HT-PyC组成的界面层
3.原位生长纳米纤维改变了热解炭的生长方向以及界面的结构,导致了NF-C/C复合材料具有更优的导热性能。不同的纳米纤维对C/C复合材料在不同方向上导热性能的影响不同。相对于平行方向的导热,CNF明显提高了C/C复合材料在垂直方向的导热性能；而相对于垂直方向的导热性能,SiCNF改性C/C复合材料在平行方向的导热性能提高更为显著。
4.通过影响炭纤维、界面和热解炭的结构,纳米纤维改性提高了C/C复合材料的硬度和弯曲强度、层间剪切强度、压缩强度及冲击韧性等力学性能。此外,纳米纤维改变了热解炭的生长方向,导致NF-C/C复合材料在不同方向上力学性能的差异。相对于平行炭纤维方向,纳米纤维改性后C/C复合材料在垂直炭纤维方向的力学性能提高更为显著。
5.纳米纤维改性对炭纤维及C/C复合材料的氧化性能的影响不同。CNF改性炭纤维因其比表面积增大、活性点增加,从而加速了氧化；而SiCNF氧化形成的SiO2保护了炭纤维,减缓了炭纤维的氧化。CNF诱导热解炭有序沉积,降低了C/C复合材料的活性,减缓了复合材料的氧化,并在短时间氧化后复合材料保持了较高的力学性能。SiCNF改性增加了炭纤维皮层碳原子的活性,导致氧化从炭纤维皮层开始,在炭纤维与基体之间形成裂纹,提供了氧的扩散通道,加速了复合材料的氧化,并导致短时间氧化后复合材料的力学性能迅速下降。
6.综合不同纳米纤维含量对改性C/C复合材料的导热、力学及氧化等性能的影响,当CNF含量为5wt%、SiCNF含量为9wt%时,纳米纤维改性C/C复合材料具有最佳的综合性能。
7.纳米纤维改性导致C/C复合材料的摩擦系数随摩擦速度的变化更为明显。纳米纤维通过影响摩擦膜的形成和破坏过程来影响复合材料的摩擦机理,从而改变复合材料的摩擦系数、影响复合材料的摩擦行为。纳米纤维还改变了C/C复合材料在摩擦过程中主要的磨损形式,从而减少了复合材料的磨损。
综上所述,利用CCVD/CVI法可以制备出微观结构可控、力学及导热性能优异的高强度高模量C/C复合材料,为C/C复合材料的进一步扩展应用范围打下了坚实的基础。
Carbon nanofibers (CNF) or silicon carbide nanofibers (SiCNF) were prepared in situ on the fiber surface of preform by catalytic chemical vapor deposition (CCVD). The preform with nanofibers was then densified to obtain carbon/carbon composites with nanofibers (NF-C/C composites) via chemical vapor infiltration (CVI). The microstructure, thermo-physical properties, mechanical properties, oxidation behavior and tribological behavior were investigated. The main research contents and results are as follows.
1. The microstructure in the skin region of carbon fibers is changed during the preparation of catalysts and nanofibers. During the preparation of the catalysts, nickel particles diffuse into the skin region of carbon fiber. The carbon atoms around nickel particles rearrange and form layers of highly ordered graphite. Consequently the graphitization degree of carbon fiber is improved. During the CCVD process, the carbon atoms diffuse into the skin region of carbon fiber and nickel particles are released from carbon fiber. Then the carbon atoms are gradually deposited on the surface of carbon fiber to form the middle-texture pyrocarbon (MT-PyC). The diffusion of SiC molecules leads to more orderly arrangement of the carbon atoms around SiC in the skin region of carbon fiber.
2. During the CVI process, nanofibers induce the formation of high-texture (HT) PyC, and result in the formation of the interface layer between carbon fiber and matrix. PyC coverd on CNFs is HT-PyC, and there is a interface layer between fiber and matrix consists of MT-PyC and CNF+HT-PyC. MT-PyC is first covered on the SiCNF surface, which is followed by HT-PyC. The interface layer between carbon fibers and matrix is composed by SiCNFs, MT-PyC and HT-PyC.
3. The in situ grown NF leads to the change of growth direction of PyC and the interfacial structure, which results in the better thermal conductivity of the NF-C/C composites compared with C/C composites. Modified with different nanofibers, the thermal conductivity of C/C composites is different in different direction. The thermal conductivity of CNF-C/C composites increases more significantly in the direction perpendicular to carbon fiber than the direction parallel to fiber. However, the thermal conductivity of SiCNF-C/C composites increases more significantly in the parallel direction than in the perpendicular direction.
4. Modified by nanofibers, the hardness, flexural strength, interlaminar shear strength, compressive strength and impact toughness of C/C composites is significantly improved. In addition, the growth direction of PyC which was changed by NF made different changes of the mechanical properties of NF-C/C composites in different directions. The mechanical properties of NF-C/C composites have been improved more significantly in the perpendicular direction compared with the parallel direction.
5. The effects of nanofibers on the oxidation behavior of carbon fibers and C/C composites are different. The in situ grown CNFs lead to the increase of the specific surface area and the active sites of carbon fiber, which can accelerate the oxidation of carbon fiber. On the other hand, the oxidation of SiCNFs forms a layer of SO2which can protect the carbon fiber from oxidation. Moreover, CNFs induce to orderly deposition of PyC, which decreases the activity of NF-C/C composites. Therefore, the oxidation of CNF-C/C composites becomes slowly. At the same time, CNF-C/C composites retain a high percentage of mechanical properties after oxidation in short time. The existence of SiCNF improves the activity of carbon fibers. As a result, the oxidation of SiCNF-C/C composites was initiated from the skin region of carbon fiber which leads to the formation of cracks between carbon fiber and matrix. C/C composites can be oxidized quicker as oxygen can diffuse from the cracks. Meanwhile, the mechanical properties of SiCNF-C/C is deteriorated markedly.
6. Taking the reasonable consideration of the effect of nanofiber content on the thermal conductivity, mechanical properties and oxidation behavior of C/C composites, the NF-C/C composites with5wt%CNF or9wt%SiCNF have the best performances.
7. The existence of nanofibers changes the friction coefficient with the increase of the friction speed more obviously. The nanofibers change of friction coefficient and the friction curve of C/C composites through affecting the formation and destruction of the frictional films during the friction process. Meanwhile, the main wear mode of C/C composites modified by nanofiber was changed, and the wear of the NF-C/C composites decreases.
In a word, the CNF-C/C and SiCNF-C/C composites can be prepared by CCVD/CVI technique, with the microstructure of composites being controlled and the excellent properties of thermal conductivity and mechanical; it was benefit to expand application of C/C composites in the further.
1.原位生长纳米纤维影响了炭纤维皮层结构的变化。在制备催化剂时,镍颗粒通过扩散进入炭纤维皮层,导致周围的碳原子重新排列,形成大微晶尺寸的高度有序石墨层,提高了炭纤维的石墨化度。在CCVD过程中,镍颗粒通过碳原子或碳化硅的内扩散从炭纤维皮层脱出。碳原子进入炭纤维皮层后修复炭纤维皮层的结构,并逐渐沉积在炭纤维表面形成中织构热解炭(MT-PyC)；碳化硅进入炭纤维皮层后,导致周围碳原子更加有序地排列。
2.纳米纤维诱导形成高织构热解炭(HT-PyC),并导致炭纤维与炭基体之间形成了一层界面层。包覆在CNF表面的PyC以HT-PyC的形式存在,并且在炭纤维与基体之间形成一层依次由MT-PyC、 CNF+HT-PyC组成的界面层；而包覆在SiCNF表面的PyC以MT-PyC和HT-PvC两种形式存在,MT-PyC介于SiCNF和HT-PvC之间,并在炭纤维与基体之间形成了一层由MTYUPvC、SiCNF以及HT-PyC组成的界面层
3.原位生长纳米纤维改变了热解炭的生长方向以及界面的结构,导致了NF-C/C复合材料具有更优的导热性能。不同的纳米纤维对C/C复合材料在不同方向上导热性能的影响不同。相对于平行方向的导热,CNF明显提高了C/C复合材料在垂直方向的导热性能；而相对于垂直方向的导热性能,SiCNF改性C/C复合材料在平行方向的导热性能提高更为显著。
4.通过影响炭纤维、界面和热解炭的结构,纳米纤维改性提高了C/C复合材料的硬度和弯曲强度、层间剪切强度、压缩强度及冲击韧性等力学性能。此外,纳米纤维改变了热解炭的生长方向,导致NF-C/C复合材料在不同方向上力学性能的差异。相对于平行炭纤维方向,纳米纤维改性后C/C复合材料在垂直炭纤维方向的力学性能提高更为显著。
5.纳米纤维改性对炭纤维及C/C复合材料的氧化性能的影响不同。CNF改性炭纤维因其比表面积增大、活性点增加,从而加速了氧化；而SiCNF氧化形成的SiO2保护了炭纤维,减缓了炭纤维的氧化。CNF诱导热解炭有序沉积,降低了C/C复合材料的活性,减缓了复合材料的氧化,并在短时间氧化后复合材料保持了较高的力学性能。SiCNF改性增加了炭纤维皮层碳原子的活性,导致氧化从炭纤维皮层开始,在炭纤维与基体之间形成裂纹,提供了氧的扩散通道,加速了复合材料的氧化,并导致短时间氧化后复合材料的力学性能迅速下降。
6.综合不同纳米纤维含量对改性C/C复合材料的导热、力学及氧化等性能的影响,当CNF含量为5wt%、SiCNF含量为9wt%时,纳米纤维改性C/C复合材料具有最佳的综合性能。
7.纳米纤维改性导致C/C复合材料的摩擦系数随摩擦速度的变化更为明显。纳米纤维通过影响摩擦膜的形成和破坏过程来影响复合材料的摩擦机理,从而改变复合材料的摩擦系数、影响复合材料的摩擦行为。纳米纤维还改变了C/C复合材料在摩擦过程中主要的磨损形式,从而减少了复合材料的磨损。
综上所述,利用CCVD/CVI法可以制备出微观结构可控、力学及导热性能优异的高强度高模量C/C复合材料,为C/C复合材料的进一步扩展应用范围打下了坚实的基础。
Carbon nanofibers (CNF) or silicon carbide nanofibers (SiCNF) were prepared in situ on the fiber surface of preform by catalytic chemical vapor deposition (CCVD). The preform with nanofibers was then densified to obtain carbon/carbon composites with nanofibers (NF-C/C composites) via chemical vapor infiltration (CVI). The microstructure, thermo-physical properties, mechanical properties, oxidation behavior and tribological behavior were investigated. The main research contents and results are as follows.
1. The microstructure in the skin region of carbon fibers is changed during the preparation of catalysts and nanofibers. During the preparation of the catalysts, nickel particles diffuse into the skin region of carbon fiber. The carbon atoms around nickel particles rearrange and form layers of highly ordered graphite. Consequently the graphitization degree of carbon fiber is improved. During the CCVD process, the carbon atoms diffuse into the skin region of carbon fiber and nickel particles are released from carbon fiber. Then the carbon atoms are gradually deposited on the surface of carbon fiber to form the middle-texture pyrocarbon (MT-PyC). The diffusion of SiC molecules leads to more orderly arrangement of the carbon atoms around SiC in the skin region of carbon fiber.
2. During the CVI process, nanofibers induce the formation of high-texture (HT) PyC, and result in the formation of the interface layer between carbon fiber and matrix. PyC coverd on CNFs is HT-PyC, and there is a interface layer between fiber and matrix consists of MT-PyC and CNF+HT-PyC. MT-PyC is first covered on the SiCNF surface, which is followed by HT-PyC. The interface layer between carbon fibers and matrix is composed by SiCNFs, MT-PyC and HT-PyC.
3. The in situ grown NF leads to the change of growth direction of PyC and the interfacial structure, which results in the better thermal conductivity of the NF-C/C composites compared with C/C composites. Modified with different nanofibers, the thermal conductivity of C/C composites is different in different direction. The thermal conductivity of CNF-C/C composites increases more significantly in the direction perpendicular to carbon fiber than the direction parallel to fiber. However, the thermal conductivity of SiCNF-C/C composites increases more significantly in the parallel direction than in the perpendicular direction.
4. Modified by nanofibers, the hardness, flexural strength, interlaminar shear strength, compressive strength and impact toughness of C/C composites is significantly improved. In addition, the growth direction of PyC which was changed by NF made different changes of the mechanical properties of NF-C/C composites in different directions. The mechanical properties of NF-C/C composites have been improved more significantly in the perpendicular direction compared with the parallel direction.
5. The effects of nanofibers on the oxidation behavior of carbon fibers and C/C composites are different. The in situ grown CNFs lead to the increase of the specific surface area and the active sites of carbon fiber, which can accelerate the oxidation of carbon fiber. On the other hand, the oxidation of SiCNFs forms a layer of SO2which can protect the carbon fiber from oxidation. Moreover, CNFs induce to orderly deposition of PyC, which decreases the activity of NF-C/C composites. Therefore, the oxidation of CNF-C/C composites becomes slowly. At the same time, CNF-C/C composites retain a high percentage of mechanical properties after oxidation in short time. The existence of SiCNF improves the activity of carbon fibers. As a result, the oxidation of SiCNF-C/C composites was initiated from the skin region of carbon fiber which leads to the formation of cracks between carbon fiber and matrix. C/C composites can be oxidized quicker as oxygen can diffuse from the cracks. Meanwhile, the mechanical properties of SiCNF-C/C is deteriorated markedly.
6. Taking the reasonable consideration of the effect of nanofiber content on the thermal conductivity, mechanical properties and oxidation behavior of C/C composites, the NF-C/C composites with5wt%CNF or9wt%SiCNF have the best performances.
7. The existence of nanofibers changes the friction coefficient with the increase of the friction speed more obviously. The nanofibers change of friction coefficient and the friction curve of C/C composites through affecting the formation and destruction of the frictional films during the friction process. Meanwhile, the main wear mode of C/C composites modified by nanofiber was changed, and the wear of the NF-C/C composites decreases.
In a word, the CNF-C/C and SiCNF-C/C composites can be prepared by CCVD/CVI technique, with the microstructure of composites being controlled and the excellent properties of thermal conductivity and mechanical; it was benefit to expand application of C/C composites in the further.
引文
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