SiC/ZrB2-SiC-B4C涂层的抗氧化和耐烧蚀性能研究

碳/碳化硅复合材料(C/SiC)在使用时经常受到高温氧化和烧蚀作用。本文采用化学气相沉积(CVD)和浆料刷涂-烧结法制备了双层SiC/ZrB2-SiC-B4C涂层,对比研究了无涂层,单层SiC涂层和双层SiC/ZrB2-SiC-B4C涂层C/SiC复合材料在1500℃下的氧化和在4.2 MW/m2热流密度下的烧蚀性能。结果表明,制备态ZrB2-SiC-B4C涂层致密、完整,表面平均粗糙度约为1 μm,孔隙率约为4.2 %。在1500℃氧化30 h后,SiC/ZrB2-SiC-B4C涂层C/SiC复合材料的质量损失率约为10%,涂层表面氧化膜致密,无明显裂纹。高温烧蚀20 s后,SiC/ZrB2-SiC-B4C涂层的线烧蚀率和质量烧蚀率分别为1.0±0.3 μm/s和1.1±0.2 mg/s,与单层SiC涂层相比分别降低了75.0 %和50.0 %,SiC/ZrB2-SiC-B4C涂层烧蚀后形成的ZrO2-SiO2氧化膜可以减缓火焰对复合材料的机械剥蚀作用。     

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％.     

SiCf/SiC复合材料表面Si/Yb2Si2O7双层涂层结合强度分析

目的 通过选择合适的复合材料拉伸方向和涂层制备工艺,在SiCf/SiC复材上获得高结合强度的Si/Yb2Si2O7双层涂层.方法 采用真空等离子喷涂技术在2.5D编织的SiCf/SiC复合材料表面制备Si涂层、Si/Yb2Si2O7双层涂层.采用金相、XRD、SEM和EDS对试样进行表征,采用拉伸试验测试涂层的结合强度...     

Si/莫来石/Er_2SiO_5环境障涂层的高温氧化行为

采用化学气相沉积与等离子喷涂相结合的方法在SiC/SiC复合材料基体上制备了Si/莫来石/Er2Si O5环境障涂层。采用扫描电镜(SEM)、能谱分析仪(EDS)与X射线衍射仪(XRD)分析其结构变化,通过氧化试验研究涂层在1350℃与1500℃下的高温氧化行为。结果表明:Si/莫来石/Er2Si O5环境障涂层可在1350℃长时间使用,在1500℃短时间使用。涂层在不同高温下的氧化失效机理不同。1350℃时,涂层氧化失效主要是由于涂层材料与基体材料热膨胀不匹配使涂层中产生了垂直于表面的裂纹,裂纹成为元素扩散通道,加速环境中O元素扩散至粘结层与基体并将其氧化,降低了涂层与基体之间的粘结强度,从而导致涂层脱落。1500℃时,涂层氧化失效主要是元素快速扩散、反应生成大量的气泡状玻璃态物质所致。     

W-SiC-C/C复合材料制备及等离子烧蚀性能

目的提高C/C复合材料在超高温下的抗烧蚀性能。方法采用化学气相沉积法,在C/C复合材料表面制备SiC过渡层,然后以惰性气体保护等离子喷涂工艺在带有SiC过渡层的C/C材料表面制备W涂层,研究所制备的W-SiC-C/C复合材料的微观形貌与结构特征。以200 kW超大功率等离子焰流,考核W-SiC-C/C材料的抗烧蚀性能,并与无涂层防护的C/C材料进行对比分析。结果W涂层主要为层状的柱状晶结构。W涂层与SiC过渡层、过渡层与基体界面呈镶嵌结构,结合良好。SiC过渡层阻止了W、C元素相互迁移与反应。在驻点压力为4.5 MPa、温度约5000 K、热流密度为36 MW/m²的烧蚀条件下,当烧蚀时间小于10 s时,涂层对C/C材料起到了较好的保护作用,W涂层发生氧化烧蚀,基体未发现烧蚀,平均线烧蚀率为0.0523 mm/s;当烧蚀时间超过15 s后,涂层防护作用基本失效,基体C/C材料发生烧蚀现象。结论以W涂层、SiC过渡层为防护的C/C复合材料,能够适用于短时间超高温的烧蚀环境,如固体火箭发动机等。W涂层的熔融吸热、氧化耗氧以及SiC过渡层的氧化熔融缓解涂层热应力和氧扩散阻碍的联合作用,提高了C/C材料的抗烧蚀性能。     

ZrB2-MoSi2/SiC涂层C/C复合材料的制备及氧化性能（英文）

为了提高C/C复合材料的抗氧化性,在C/C复合材料基体上制备了ZrB2-MoSi2/SiC涂层。采用包埋法制备SiC中间层,采用喷涂法制备ZrB2-MoSi2外涂层。用XRD和SEM分别分析、测试所制备涂层的物相组成和显微结构,研究涂层复合材料的高温抗氧化性能。结果表明:C/C复合材料的外涂层由ZrB2、MoSi2和SiC三相组成;在1273K和1773K下分别氧化30h和10h后ZrB2-MoSi2/SiC涂层试样的质量损失分别为5.3%和3.0%,涂层表面长有纳米SiC晶须。C/C复合材料ZrB2-MoSi2/SiC涂层具有自愈合特性和良好的高温抗氧化性能。     

碳纤维CVD SiC涂层对C/SiC复合材料力学性能的影响

采用CVD PIP工艺制备了SiC涂层碳纤维增强SiC复合材料(C/SiC),研究了碳纤维表面CVD SiC涂层的形貌以及涂层对C/SiC复合材料力学性能的影响.结果表明CVD SiC涂层处理可以填补纤维表面上的沟槽和缺陷,使纤维表面变得光滑,从而使C/SiC复合材料的力学性能有很大提高,碳纤维经过CVD SiC 1 h涂层处理的C/SiC复合材料的力学性能最好,弯曲强度达到511.5 MPa,断裂韧性达到20.8 MPa·m1/2.     

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。     

碳/碳复合材料SiC/W-Al-Si涂层微观结构及抗氧化性能

分别采用包埋法、料浆法在碳/碳（C/C）复合材料表面制备了碳化硅（SiC）内涂层、W-Al-Si合金外涂层,借助XRD和SEM分析了所得涂层的物相组成和微观结构,并测试了带有单一SiC涂层、SiC/W-Al-Si双涂层碳/碳复合材料试样在1500℃静态空气中的抗氧化性能。结果表明：富Si的SiC内涂层结构疏松,仅能为碳/碳基体提供数小时的防氧化保护;W-Al-Si合金外涂层主要由WSi2和W（Si,Al）2两相组成;SiC/W-Al-Si双涂层厚度约为100μm,其抗氧化性能明显优于单一SiC涂层,氧化19 h后涂层试样的质量损失未超过5%;有望进一步通过优化W-Al-Si外涂层料浆比例,避免因为与SiC内涂层热膨胀不匹配而产生透性裂纹,从而发挥出超过19 h后SiC/W-Al-Si双涂层的氧化防护潜力。     

SiC涂层对C/C复合材料高温氧乙炔焰烧蚀性能影响

采用化学气相反应法在C/C复合材料表面制备抗氧化SiC涂层,借助X射线衍射仪、扫描电镜及能谱等分析手段,研究涂层的结构;通过氧乙炔焰烧蚀试验考察SiC涂层对C/C复合材料高温耐烧蚀性能影响。结果表明:SiC涂层可明显提高C/C复合材料的高温短时耐烧蚀性能,经过20 s的高温氧乙炔焰烧蚀后,C/C复合材料试样的线烧蚀率和质量烧蚀率分别为13μm/s和6.6 mg/s,SiC涂层试样的线烧蚀率和质量烧蚀率分别为22μm/s和0.5 mg/s;在烧蚀中心区,涂层试样的烧蚀以升华分解为主,同时还伴有氧化烧蚀和微区机械剥蚀;在烧蚀过渡区,涂层的烧蚀机制以热氧化和燃气冲刷为主;而在烧蚀边缘区,涂层的烧蚀则主要表现为弱氧化烧蚀。     

Influence of preparation temperature on the oxidation resistance and mechanical properties of C/SiC coated C/C composites

A C/SiC oxidation resistance coating was prepared on carbon/carbon (C/C) composites by slurry and pack cementation. The microstructure, oxidation resistance and mechanical properties of C/SiC coating prepared from 1773 to 2573 K were investigated. With the increase of the preparation temperature, the oxidation resistance of C/SiC coating increases, however, the flexure strength decreases gradually. The preparation of C/SiC coating on C/C composites results in the fracture behavior of C/C composites changing from pseudo-plastic to brittle failure model. The decrease of flexure strength is mainly attributed to the decrease of C/C matrix’ flexure strength at high temperature.     

Effect of Thermal Shock and Oxidation on Mechanical Property of Carbon/Carbon Composites with a Silicide Coating

A SiC whisker-toughened MoSi2-SiC-Si coating was prepared on carbon/carbon (C/C) composites surface by a two-step technique of slurry and pack cementation, and the effects of thermal shock and oxidation on the mechanical property of the coated C/C were studied. The flexural strength of C/C composites was improved by 6.8% after coated by SiC whisker-toughened MoSi2-SiC-Si. After thermal cycle between 1773 K and room temperature in air for 10 times, the mass loss of the coated sample was 5.08% and the percent...     

多孔体制备工艺对C/C-SiC复合材料弯曲性能的影响

以针刺整体炭毡为坯体,采用CVD和树脂浸渍／炭化混合法增密制备了4种C／C多孔体,然后熔硅浸渗C／C多孔体制备了C／C-SiC复合材料;研究了不同炭涂层、高温热处理对C／C-SiC复合材料弯曲强度和断裂方式的影响。结果表明：热解炭涂层可减少制备过程中炭纤维的损伤,具有适中的界面结合强度,使复合材料的弯曲强度达到161．5MPa,表现出良好的“假塑性”;适当选择高温热处理工艺可制备弯曲性能较高,具有一定“假塑性”的C／C-SiC复合材料。     

HfB2/SiC as a protective coating for 2D Cf/SiC composites: Effect of high temperature oxidation on mechanical properties

In the field of thermal shielding for aerospace applications C_f/SiC composites are raising great interest, provided that they are protected from oxidation by suitable coatings. Conversely, ultra high temperature ceramics, and in particular HfB₂, are among the best oxidation resistant materials known. A coating made of a HfB₂/SiC composite (20% weight SiC) was tested as an oxidation protection on a C_f/SiC composite. The composite was produced by Polymer Impregnation Pyrolysis (PIP), which is a simple and low cost method; the coating was applied by painting a slurry on the surface of the composite and by heat treating. The thermal behaviour was studied by thermo-gravimetric analysis, and mechanical tests were conducted before and after oxidation. The HfB₂/SiC composite seems to effectively protect the underlying C_f/SiC composite, with a mechanical strength reduction of only 20% after 30 min at 1600 °C, even if some weight loss due to partial carbon fibre damage is observed. A first analysis of thermal cycling in oxidizing environment suggested that the HfB₂/SiC coating reduces continual damage thanks to the sealing effect of the glassy surface layer.     

高温处理对不同浆料制备C/SiC复合材料的影响

以先驱体浸渍裂解(PIP)工艺制备的C/SiC复合材料为研究对象,考察了聚碳硅烷/二甲苯(PCS/Xylene)和聚碳硅烷/二甲苯/碳化硅粉(PCS/Xylene/SiC)两种浆料对C/SiC材料耐高温性能的影响.研究发现:在1600 ℃惰性气氛保护下高温处理1 h后,PCS/xylene/SiC制备的材料失重较大,达4.67%.弯曲强度在高温处理前后的保留率较高,高温处理后其强度达464.1 MPa,但模量下降明显.高温处理使C/SiC材料的增韧机制发生改变,PCS/Xylene中添加SiC改变了材料的界面结构.结果表明:两种不同的浸渍浆料对C/SiC材料的耐高温性能有着较明显的影响.     

Strengthening of C/SiC Composites by Electrophoretic Deposition of CNTs on a SiC Coating

The current study reports the enhancement of mechanical properties of carbon fiber-reinforced silicon carbide ceramic matrix composites (C/SiC CMCs) by the application of a carbon nanotube/silicon carbide (CNT/SiC) coating. CNTs were deposited on the surfaces of C/SiC composites using electrophoretic deposition (EPD), after which infiltration by SiC was achieved through a chemical vapor infiltration process. An EPD duration of 5 min was associated with a 40% increase in the ultimate flexural strength relative to that of composites with a pure SiC coating. The observed enhancement was rationalized by the microstructural observations of SiC infiltration into the porous CNT morphology and the subsequent formation of CNT/SiC layers on the surfaces of the composites and by the inherent toughness of the SiC whiskers. The flexural strength decreased with EPD durations greater than 5 min due to the formation of thick CNT meshes, which decreased the open porosity and thereby obstructed further SiC infiltration. This is a viable methodology for the improvement of mechanical properties of CMCs by the introduction of a ceramic coating containing CNT.     

Influence of SiC nanowires on the properties of SiC coating for C/C composites between room temperature and 1500 °C

To prevent carbon/carbon (C/C) composites from oxidation between room temperature and 1500 °C, a dense SiC nanowire-toughened SiC oxidation resistant coating was prepared by a two-step technique composed of chemical vapor deposition and pack cementation. SiC nanowires could effectively baffle the propagation of the microcracks and avoid the formation of the through-thickness microcracks in the original coating. The results indicated that, after introducing SiC nanowires, the coefficient of thermal expansion of the coating was decreased between 100 and 1500 °C, and the oxidation protective ability for the coated C/C composites was improved largely between room temperature and 1500 °C.     

Oxidation and ablation resistance of ZrB2–SiC–Si/B-modified SiC coating for carbon/carbon composites

ZrB₂–SiC–Si/B-modified SiC coating was prepared on the surface of carbon/carbon (C/C) composites by two-step pack cementation. The coating could efficiently provide protection for C/C composites from oxidation and ablation. The improvement of oxidation resistance was attributed to the self-sealing property of the multilayer coating. A dense glassy oxide layer could afford the high temperature up to 2573 K and efficiently protect C/C composites from ablation.     

Fabrication of Y2Si2O7 coating and its oxidation protection for C/SiC composites

Yttrium silicate (Y₂Si₂O₇) coating was fabricated on C/SiC composites through dip-coating with silicone resin + Y₂O₃ powder slurry as raw materials. The synthesis, microstructure and oxidation resistance and the anti-oxidation mechanism of Y₂Si₂O₇ coating were in–estigated. Y₂Si₂O₇ can be synthesized by the pyrolysis of Y₂O₃ powder filled silicone resin at mass ratio of 54.2:45.8 and 800 °C in air and then heat treated at 1400 °C under Ar. The as-fabricated coating shows high density and fa–orable bonding to C/SiC composites. After oxidation in air at 1400, 1500 and 1600 °C for 30 min, the coating-containing composites possess 130%–140% of original flexural strength. The desirable thermal stability and the further densification of coating during oxidation are responsible for the excellent oxidation resistance. In addition, the formation of eutectic Y–Si–Al–O glassy phase between Y₂Si₂O₇ and Al₂O₃ sample bracket at 1500 °C is disco–ered.     

Effect of C/SiC Volume Ratios on Mechanical and Oxidation Behaviors of Cf/C-SiC Composites Fabricated by Chemical Vapor Infiltration Technique

C/SiC volume ratios in carbon fiber-reinforced carbon-silicon carbide (C_f/C-SiC) composites may influence greatly mechanical and oxidation properties of the composites, but have not been well investigated yet. Herein, C_f/C-SiC composites with different C/SiC volume ratios were fabricated by chemical vapor infiltration (CVI) technique through alternating the thickness of a pyrocarbon (PyC) interlayer. The composites with C/SiC volume ratios of 0.37 and 0.84 exhibited the better comprehensive mechanical properties. The CS0.37 showed the highest flexural strength of 340.6 MPa, and CS0.84 had the maximum tensile strength of 139.1 MPa. The excellent mechanical properties were closely related to the relatively low C/SiC volume ratios and porosities, optimum interfacial bonding and reduced matrix micro-cracks. The composite with a low C/SiC volume ratio of 0.10 showed the best anti-oxidation performance due to its high SiC content. The oxidation mechanisms at 1100 °C and 1400 °C were discussed by considering the effect of the C/SiC volume ratios, pores and matrix micro-cracks, oxidation of carbon phase and SiC.