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。     

等离子喷涂制备C/C复合材料SiC涂层的驻点烧蚀性能

目的在C/C复合材料表面制备SiC涂层,提高C/C复合材料抗烧蚀性能。方法采用真空等离子喷涂技术在C/C复合材料表面制备纯Si涂层,在惰性气氛保护下对涂层高温热处理,纯Si涂层与C元素在高温下反应,原位生成SiC涂层。利用电弧加热器在不同烧蚀温度下,分别考核涂层的驻点烧蚀性能,并采用OM、SEM、EDS和XRD等对烧蚀前后的微观形貌和物相成分进行分析。结果在C/C复合材料表面制备了致密的SiC涂层,涂层中没有明显的裂纹存在,并在涂层下方产生较深的渗透区域,深度超过涂层厚度。制备的SiC涂层在1400℃下烧蚀50 s,涂层完整,具有良好的驻点烧蚀性能;在1600℃和1650℃下烧蚀50 s,涂层部分剥落,C/C复合材料基体产生烧蚀。结论 SiC涂层在高温下氧化成Si O2玻璃态膜,并覆盖在C/C复合材料表面,对基体具有良好的保护作用。随着烧蚀温度的提高,在超音速气流的冲刷下,由于热膨胀系数不匹配和SiC主动氧化的原因,涂层在烧蚀面边缘出现剥落,且剥落现象越来越严重,涂层失去对C/C基体的保护作用,烧蚀性能下降。     

铌合金表面MoSi2-B4C复合涂层的快速烧结制备及高温氧化行为

以Mo-Si-B4C混合粉末为涂层原料,采用放电等离子烧结在铌合金表面原位反应烧结制备MoSi2-B4C复合涂层,研究涂层组织形成过程及界面反应特征,考察涂层在1450℃下的抗氧化性能。结果表明,在烧结的升温阶段,MoSi2相就已完全形成,而在保温的初期阶段,部分B4C颗粒又与邻近的MoSi2反应生成了SiC和Mo2B5。烧结过程中,涂层中的Si和B向基体合金扩散,形成了由NbSi2 + NbB外层和Nb5Si3内层组成的互扩散区。涂层在1450℃至少100h内可有效保护基体,表面生成了致密的SiO2-B2O3氧化膜,而互扩散区内NbB的存在有效阻碍了氧化过程涂层中Si的内扩散。     

Si/Zr质量比对SiC/ZrC涂层微观结构及其抗氧化性能的影响

采用反应熔体浸渗工艺在C/C复合材料表面制备了SiC和SiC/ZrC抗氧化涂层,并利用XRD、SEM和EDS等分析手段研究了浸渗粉料中Si/Zr质量比对抗氧化涂层的相组成和微观结构的影响,考察了SiC和SiC/ZrC涂层在1 400℃静态空气气氛中的抗氧化性能,初步探讨了SiC/ZrC涂层的抗氧化机制。研究结果表明,随着浸渗粉料中Si/Zr质量比由4.5∶1.5降至2∶4,制得的SiC/ZrC涂层表面涂层致密性呈现先增后降的趋势,而涂层厚度则逐渐减小。当Si/Zr质量比为3∶3时,制得SiC/ZrC涂层C/C复合材料表现出优良的抗氧化性能,在空气气氛中1 400℃氧化6h后增重0.5%左右,而SiC涂层C/C复合材料在相同条件下氧化5h后失重率达到26.71%。SiC/ZrC涂层优异的抗氧化性能与其表面形成的一层致密、连续的ZrSiO4-SiO2-ZrO2玻璃膜有关。     

HfB_2-WB_2-Si/SiC-SiC_(NW)复合涂层的制备及其抗氧化性能

为解决C/C复合材料的高温易氧化问题,依次采用前驱体浸渍裂解、反应熔体浸渗和料浆涂刷法在C/C复合材料表面制备HfB_2-WB_2-Si/SiC-SiC_(NW)复合涂层。考察Si C涂层、HfB_2-WB_2-Si/SiC涂层和HfB_2-WB_2-Si/SiC-SiC_(NW)涂层C/C复合材料在1 500℃静态空气中的抗氧化性能。结果表明:HfB_2-WB_2-Si/SiC-SiC_(NW)涂层抗氧化效果优于HfB_2-WB_2-Si/Si C涂层和Si C涂层,前者试样氧化20 h后增重0.1%,后两者则分别失重0.9%和22.8%。HfB_2-WB_2-Si/SiC-SiC_(NW)涂层较好的抗氧化性能主要归因于涂层氧化形成的连续、具有较好流动性的HfSiO_4-SiO_2-WO_3复相玻璃以及SiC纳米线(SiCNW)对涂层的增韧作用,前者有效抑制了氧气向C/C复合材料基体内部的扩散,后者则使涂层内部裂纹的数量和尺寸明显减小。     

SiZr液相烧结法制备SiC-ZrC涂层对C/SiC复合材料抗氧化性能的影响

使用Si-25％Zr(质量分数)合金通过液相烧结法在C/SiC复合材料表面制备了SiC-ZrC抗氧化涂层,研究了烧结过程中涂层的相结构演化,并测试了1400℃及空气气氛下材料的抗氧化性能,分析了涂层氧化前后显微结构的变化,以及氧化对C/SiC复合材料弯曲性能的影响.结果表明,Zr元素在涂层中以ZrC相的形式存在,ZrC颗粒的引入细化了反应SiC层的组织,在氧化过程中形成致密连续的SiO2薄膜,并在氧化500 s后试样出现增重,制备了SiC-ZrC抗氧化涂层的C/SiC样品在1000 s的氧化实验后弯曲强度下降低于5％.     

反应烧结SiC制备SiC/B4C复合材料的研究

基于反应烧结SiC制备出相对密度较高的SiC/B4C复合材料,并探讨原料中C含量对SiC/B4C复合材料物相、显微结构、体积密度、力学性能的影响。结果表明,SiC/B4C复合材料的相组成为B4C、SiC、Si、B13C2和B12.97Si0.03C2。SiC/B4C复合材料的显微组织为:SiC相和B4C相均匀分布,游离Si填充在B4C相和SiC相的空隙处,且形成了连续相。随着原料中C含量的增加,复合材料的力学性能整体呈现先增加后降低的趋势。原料中C最佳添加量为10%(质量分数),对应SiC/B4C复合材料的维氏硬度、抗弯强度和断裂韧性分别为24.4GPa、361.3MPa和4.41MPa·m1/2,复合材料开口气孔率和体积密度分别为0.19%和2.58g/cm3。     

C/C复合材料表面SiC/MoSi_2涂层的组织及氧化性能研究

在C/C复合材料表面制备SiC/MoSi_2涂层,并对其物相结构及截面与表面形貌进行了表征,同时对试样抗氧化性能进行了测试。研究结果表明:SiC涂层的表面上分布着松散结合状态的瓦砾状颗粒物,形成了众多的孔洞与裂纹。SiC/MoSi_2涂层的表面包含了玻璃态与瓦砾状颗粒,有效避免了涂层表面的孔洞形成,SiC/MoSi_2涂层含有Si、SiC、MoSi_2三种物相。SiC/MoSi_2复合涂层的失重曲线位于SiC内层的下部,具有明显的防氧化效果。与SiC涂层相比,SiC/MoSi_2涂层在氧化之后形成的气泡尺寸显著降低,有效减少了氧气扩散通道。SiC/MoSi_2复合涂层从基体往涂层表面过渡时呈现出明显的梯度涂层结构。     

放电等离子烧结制备SiC/MoSi_2复合材料的显微组织、烧结行为及力学性能（英文）

以Mo、Si和SiC粉末为原料,利用放电等离子烧结技术在不同温度下制备SiC/MoSi_2复合材料,研究SiC/MoSi_2复合材料的物相组成、显微组织和力学性能,并探讨其烧结行为。结果表明:SiC/MoSi_2复合材料由MoSi_2、SiC和少量的Mo_(4.8)Si_3C_(0.6)组成,呈现细晶组织。在Si C/MoSi_2复合材料的烧结过程中,存在固相烧结至液相烧结的演变。1600°C烧结的Si C/MoSi_2复合材料表现出最好的力学性能,其维氏硬度、抗弯强度、断裂韧性分别为13.4 GPa、674 MPa和5.1 MPa·m~(1/2),比纯MoSi_2分别提高了44%、171%和82%。第二相SiC作为硬质相可以承受外加应力,并阻碍裂纹的快速扩展,有助于复合材料力学性能的提高。     

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。     

N-乙酰半胱氨酸活性炭缓释微囊对幼鼠非酒精性脂肪肝病miRNA的影响

目的: 初步研究N-乙酰半胱氨酸活性炭缓释微囊对幼鼠非酒精性脂肪肝病的保护作用,并且探讨其对miRNA及相应的靶基因的影响。方法: 采用高脂饲料喂养的方法复制幼鼠非酒精性脂肪性肝病（non-alcoholic fatty liver disease,NAFLD）模型。HE染色观察幼鼠肝组织脂肪变性程度;microRNA芯片检测肝组织的miRNA表达谱;荧光定量PCR对miRNA进行验证;采用荧光定量PCR和Western blot法对目标miRNA进行靶基因预测并进行验证。 结果: 根据检测结果,初步确定miRNA199a-5p和miRNA-378-5p是NAFLD的关键miRNA,脂蛋白脂酶（lipoprotein lipase,Lpl）是miRNA199a-5p的靶基因,固醇调节元件结合蛋白（sterol regulatory element binding proteins-1,Srebp1）、CCAAT增强子结合蛋白α（CCAAT enhancer binding protein alfa,C/EBP-α）是miRNA-378-5p的靶基因。结论: 推测N-乙酰半胱氨酸活性炭缓释微囊可能通过上调Lpl表达水平,下调Srebp1和C/EBP-α表达水平。这些基因与脂肪肝密切相关,可能对幼鼠NAFLD具有保护作用。     

不同基体炭C/C复合材料的摩擦磨损性能

以炭纤维针刺毡为预制体,采用化学气相沉积法(CVI)和结合液相浸渍树脂或沥青法制备了热解炭为粗糙层与光滑层结构的准三维C/C复合材料,并研究了这些材料在0.6 MPa的模拟刹车压力下的摩擦磨损性能与磨损机理.研究表明:基体炭为粗糙层热解炭与树脂炭的C/C复合材料摩擦表面能形成较厚且连续的自润滑摩擦膜,摩擦稳定性最好,摩擦因数适中,氧化磨损小,磨损机理主要为膜的部分脱落、氧化磨损与相对较小的磨粒磨损;基体炭为光滑层热解炭与树脂炭或沥青炭的C/C复合材料摩擦表面形成的摩擦膜较薄且不连续,摩擦稳定性差,摩擦磨损较大,磨损机制主要为膜的部分脱落、磨粒磨损与更严重的氧化磨损;随着密度的升高,C/C复合材料摩擦稳定性增加,摩擦因数增加,磨损降低;基体炭为单一沥青炭的C/C复合材料,由于没有热解炭对纤维的保护,纤维断裂多,线性磨损尤其大,磨损机理主要为大量的磨粒磨损与氧化磨损.     

Flexural destructive process of unidirectional carbon/carbon composites reinforced with in situ grown carbon nanofibers

Unidirectional carbon/carbon (C/C) composites modified with in situ grown carbon nanofibers (CNFs) were prepared by catalysis chemical vapor deposition. The effect of in situ grown CNFs on the flexural properties of the C/C composites was investigated by detailed analyses of destructive process. The results show that there is a sharp increase in the flexural load-displacement curve in the axial direction of the CNF-C/C composites, followed by a serrated yielding phenomenon similar to the plastic materials. The failure mode of the C/C composites modified with in situ grown CNFs is changed from the pull-out of single fiber to the breaking of fiber bundles. The existence of interfacial layer composed by middle-textured pyrocarbon, CNFs and high-textured pyrocarbon can block the crack propagation and change the propagation direction of the main crack, which leads to the higher flexural strength and modulus of C/C composites.     

Densification mechanism of chemical vapor infiltration technology for carbon/carbon composites

Carbon/carbon composites were fabricated using pressure-gradient chemical vapor infiltration（CVI） technology with propane （C3H6） as the carbon precursor gas and nitrogen （N2） as the carrier gas. The chemical process of deposition of pyrolytic carbon was deduced by analyzing the component of molecules in gas phase and observing the microstructure of deposition carbon. The results show that the process of deposition starts from the breakdown of C-C single bond of propene （C3H6）, and forms two kinds of active groups in the heterogeneous gas phase reaction. Afterwards, these active groups form many stable bigger molecules and deposit on carbon fiber surface. At the same time, hydrogen atoms of the bigger molecules absorbed on carbon fiber surface are eliminated and the solid pyrolytic carbon matrix is formed in the heterogeneous reaction process.     

Microstructure of a Mo-Si-C-N multi-layered anti-oxidation coating on carbon/carbon composites by fused slurry

A Mo-Si-C-N multi-layered anti-oxidation coating was in-situ fabricated by introducing nitrogen atmosphere during the fused sintering of Mo-Si slurry pre-layer on carbon/carbon composites. The phase composition and microstructure of the Mo-Si-C-N coating were character-ized by X-ray diffractometry, optical microscopy, scanning electron microscopy with energy dispersive spectroscopy, X-ray photoelectron spectroscopy, and transmission electron microscopy. The Mo-Si-C-N coating exhibited a three-layered structure. Besides the MoSi2/Si main-layer and the SiC bonding-layer, a surface layer of about 10 μm in thickness was synthesized on the coating surface. The surface layer mainly consisted of SiC nanowires and contained some Si3N4 and Si phases. SiC nanowires of 10 to 200 nm in diameter presented a terrace and distortion structure. Transmission electron microscopy indicated that the SiC nanowires grew along the preferred <111> direction. Dur-ing oxidation test, SiC nanowires transmuted into Sit2 glass, which can play an important role in improving the oxidation resistance of C/C composites.     

Anti-oxidation properties of ZrB2 modified silicon-based multilayer coating for carbon/carbon composites at high temperatures

To improve the anti-oxidation ability of silicon-based coating for carbon/carbon (C/C) composites at high temperatures, a ZrB₂ modified silicon-based multilayer oxidation protective coating was prepared by pack cementation. The phase composition, microstructure and oxidation resistance at 1773, 1873 and 1953 K in air were investigated. The prepared coating exhibits dense structure and good oxidation protective ability. Due to the formation of stable ZrSiO₄–SiO₂ compound, the coating can effectively protect C/C composites from oxidation at 1773 K for more than 550 h. The anti-oxidation performance decreases with the increase of oxidation temperature. The mass loss of coated sample is 2.44% after oxidation at 1953 K for 50 h, which is attributed to the decomposition of ZrSiO₄ and the volatilization of SiO₂ protection layer.     

The effect of partially carbonized fibers on the mechanical properties of carbon/carbon composites

The carbon/carbon (C/C) composite with satisfactory mechanical properties were obtained through introduction of partially carbonized fibers as a precursor. Applying this procedure the production cost of C/C composites may be significantly reduced. Stabilized PAN fibers were partially carbonized at temperatures ranging from 400 to 1000 °C and reinforced with phenolic resin, resole type. Cured composite were carbonized up to 1000 °C in an inert atmosphere. Monofilament tensile test strength, Young's modulus and tensile strength of partially carbonized fibers were determined. Mechanical properties of carbon/carbon composites (flexural strength and flexural modulus) determined by using three-point bending test. The effect of partially carbonized fibers on the mechanical properties of C/C composites was examined by scanning electron microscope (SEM) through analysis of the fracture surface. The C/C composite reinforced with partially carbonized fibers at 600 °C showed quite satisfactory flexural strength. This confirms assumptions that through co-carbonization of partially carbonized fibers and resin C/C composite with suitable mechanical properties could be obtained.     

Ablation resistance and thermal conductivity of carbon/carbon composites containing hafnium carbide

Ablation properties and thermal conductivity of carbon/carbon (C/C) composites containing hafnium carbide (HfC) were investigated. The C/C composites containing 6.5 wt.% HfC exhibit the best thermal conductivity and ablation resistance. The improvement of the thermal conductivity is attributed to the increased phonon–defect interaction produced by the thermal motion of CO released from the reaction of carbon and ZrO₂. High thermal conductivity of the composites can slow down the ablation of carbon. When the HfC mass fraction is greater than 6.5 wt.%, cracks generated act as diffusion channels for an oxidizing atmosphere and thus accelerate the ablation of the composites.     

耐烧蚀超高温陶瓷改性C/C复合材料的研究进展

炭/炭(C/C)复合材料在高温含氧环境中易氧化烧蚀的问题影响了其在航空航天领域的应用,引入超高温陶瓷能有效地提高其超高温耐烧蚀性能。介绍和分析了化学气相渗透、先驱体浸渍裂解、反应熔渗等基体改性工艺及其优缺点;综述了近年来C/C复合材料基体改性提高其超高温抗烧蚀性能的最新研究进展;并评述了国内在提高C/C复合材料超高温抗烧蚀性能方面取得的一些成果;最后,提出了提高C/C复合材料超高温长时抗烧蚀性能的潜在发展方向。     

C/C复合材料与TC4钎焊接头的组织与断裂形式分析

在钎焊时间10 min,钎焊温度820～900℃的条件下,采用AgCu钎料对C/C复合材料和TC4进行了钎焊试验.利用扫描电镜、X射线衍射分析仪、EDS能谱分析仪对接头的界面组织及断口形貌进行了研究.结果表明,C/C复合材料与TC4连接接头的界面结构为C/C复合材料/TiC C/TiCu/Ag(s.s) Cu(s.s) Ti3Cu4/Ti3Cu4/TiCu/Ti2Cu/Ti2Cu Ti(s.s)/TC4.由压剪试验测得的接头抗剪强度可知,在钎焊温度850 ℃,保温时间10 min的钎焊条件下,接头获得的最高抗剪强度达到38 MPa.接头的断口分析表明,接头的断裂位置与被连接处碳纤维方向和钎焊温度有关.当碳纤维轴平行于连接面时,断裂发生在复合材料中.当碳纤维轴垂直于连接面时,若钎焊温度较低,断裂发生在C/C复合材料/钎料界面处;若钎焊温度较高,断裂主要发生在C/C复合材料/钎料界面和钎料/TC4界面处.