包埋浸渗/气相沉积二步法在C/C复合材料表面制备SiC涂层

采用包埋浸渗法和化学气相沉积(CVD)法相结合在炭/炭(C/C)复合材料表面制备了SiC涂层, 借助扫描电镜、能谱分析以及X射线衍射等检测手段对涂层的微观组织形貌、元素分布和物相组成进行了观察与分析. 结果表明:包埋法制备的SiC涂层与C/C复合材料基体的界面处形成了梯度过渡层, CVD法制备的涂层十分致密, 有效填充了包埋SiC涂层中的孔隙, 因此, 二步法制备的SiC涂层具有良好的防氧化性能, 涂层试样在1500℃静态空气中氧化60h失重率仅为2.01%. 试样失重的主要原因是其在高低温热循环过程中氧气从涂层中的微裂纹扩散至基体表面, 从而引起基体氧化所致.     

炭/炭复合材料用SiC-Glass涂层的高温氧化机理

采用包埋法和预涂-烧结法相结合的组合工艺在炭/炭(C/C)复合材料表面制得SiC-Glass复合涂层, 并借助X射线衍射仪(XRD)和扫描电镜(SEM)对该复合涂层进行了表征, 研究了涂层C/C试样在不同温度下的氧化动力学规律。结果表明: 复合涂层具有双层结构, 包埋SiC内层由β-SiC相和少量游离硅相组成, 外层由MoSi₂颗粒掺杂的硼硅酸盐玻璃构成; 内外层之间结合紧密; 在1300~1600℃的空气气氛中, SiC-Glass涂层表现出良好的抗氧化性能, 其氧化激活能为118.1kJ/mol, 氧化主要受控于氧在Glass层中的体扩散速率; 在1600℃空气气氛中氧化65h后, SiC-Glass涂层C/C试样的氧化失重率仅为1.02%。      

C/C复合材料SiC/W-Mo-Si抗氧化复合涂层研究

为了防止C/C复合材料高温氧化,采用两步包埋法在其表面制备SiC/W-Mo-Si抗氧化复合涂层,研究了促渗剂B2O3和制备温度对该复合涂层在1500℃静态空气中防氧化能力的影响.结果表明,在第一步包埋粉料中含有B2O3会增加SiC过渡层缺陷含量,降低单一SiC涂层和复合涂层抗氧化性能.第二步包埋制备外涂层的适宜温度为2 250℃,所形成的复合涂层结构致密,有良好的自愈性和优异的抗氧化性能.能在1 500℃保护C/C复合材料抗氧化170 h以上.产生穿透性裂纹是涂层失效的主要原因.     

等离子喷涂ZrC基涂层逐道逐层沉积残余应力模拟与实验验证

采用商用ANSYS14.5软件, 依据复合梁增层力学模型, 采用逐道逐层累积模型模拟了C/C复合材料表面等离子喷涂ZrC基涂层沉积残余应力的特征, 分析了SiC过渡层、第二相(SiC, MoSi₂)和涂层厚度对ZrC基涂层残余应力的影响, 并进行了实验验证。结果表明, SiC过渡层有效缓解了涂层与基体的热失配应力。涂层体系的应力随着涂层厚度的增加逐渐减小, 符合应力松弛和叠加规律。在涂层内部的径向应力以拉应力为主, 基体中主要为压应力, 且在界面边缘存在压应力集中的极限区域, 易使涂层产生裂纹并沿界面扩展。该模拟采用逐道逐层累积的方法更逼近实际喷涂过程, 能更准确预测涂层的残余应力。     

炭/炭复合材料SiC/Mo(Si_x、Al_(1-x))_2抗氧化涂层(英文)

为了提高炭/炭(C/C)复合材料的高温抗氧化性能,应用多相反应技术在C/C复合材料表面制备SiC/Mo(Six、Al1-x)2复合涂层。利用扫描电镜、电子能谱、X射线衍射仪等测试手段对涂层材料的微观结构和物相组成进行分析,同时研究涂层C/C复合材料在超音速气流中的抗氧化性能。结果表明,C/C复合材料表面形成的抗氧化涂层显示出明显的双层结构,从外向内分别为Mo(Six、Al1-x)2与SiC的复合层和纯SiC层,同时有少量的Mo4.8Si3C0.6存在于涂层中。在温度为1800K、气体速率1500m/s的超音速气流中氧化冲刷96 s,以及在2550 K和室温下热循环24次的测试条件下,制备的SiC/Mo(Six、Al1-x)2涂层材料均未发生破坏现象。涂层材料优良的抗氧化性能和抗热震性能主要归因于基体C/C复合材料的高强度以及在氧化过程中材料表面形成的连续稳定的SiO2和Al2O3玻璃相。     

反应法制备硼化锆耐超高温涂层

为了提高C/SiC复合材料的超高温抗烧蚀性能,以锆粉、硼粉和酚醛树脂为原料,通过泥浆涂刷后高温烧结的方法在C/SiC表面制备了ZrB2涂层,研究了涂层的烧结反应过程,并对其组成、结构和抗烧蚀性能进行了表征.结果表明:1200℃前Zr先与碳反应生成ZrC,然后在1400～1600℃时ZrC与B反应生成ZrB2.浆料配比为n(Zr):n(B):n(C)=1.0:1.5:1.0时,1600℃制备的涂层由ZrB2、少量的ZrC及ZrO2组成.氧乙炔焰烧蚀60s后,由于ZrB2氧化形成了ZrO2熔融层,涂层后的C/SiC复合材料的线烧蚀率几乎为零,而未涂层的C/SiC复合材料的线烧蚀率为0.064mm/s.     

SiC/PyC复合涂层碳纤维微观结构及氧化行为研究

采用两步法在碳纤维表面制备了碳化硅/热解碳(SiC/PyC)复合涂层,PyC内涂层的制备采用等温化学气相渗透法,SiC外涂层的制备采用碳热还原法.借助X射线衍射、场发射扫描电镜、透射电镜分析了SiC/PyC复合涂层碳纤维的物相组成以及微观结构,利用热重分析研究了SiC/PyC复合涂层、PyC涂层以及无涂层碳纤维的氧化行为.结果表明,在碳纤维表面制备的SiC/PyC复合涂层连续致密、厚度均匀,PyC内涂层厚度约为200nm,SiC外涂层厚度约为160nm,SiC层中存在大量孪晶面高度有序的SiC孪晶.SiC/PyC复合涂层能够有效地改善碳纤维的抗氧化性能,较无涂层碳纤维起始氧化温度提高了近250℃.     

用碳化稻壳制备碳/碳复合材料的SiC涂层

以碳化稻壳为原料,采用包埋法在C/C复合材料表面制备了SiC涂层.用X衍射仪、扫描电镜及能谱分析仪对SiC涂层晶相、微观形貌及成分进行了分析,并探讨了涂层的形成机理.研究结果表明:所制备的SiC涂层呈网状结构,以β-SiC为主,并含有少量的α-SiC,纯度较高;碳化稻壳中含有的纳米级的SiO2微晶是低温下制备SiC涂层及涂层呈网状结构的主要原因.     

等离子熔覆ZrB_2-ZrC/Fe复合涂层组织及耐磨性

采用等离子熔覆技术,以Zr、Fe、B_4C混合粉末为原料,在Q235低碳钢表面原位反应合成了ZrB_2和ZrC增强的Fe基复合涂层,分析了ZrB_2-ZrC/Fe涂层的物相组成和组织结构,并进行了硬度、耐磨性对比试验,探讨了物相和组织结构的形成过程及磨损机制。结果表明:涂层主要物相为ZrB_2、α-Fe、ZrC、Fe_2B和Fe_3C,其中ZrB_2呈现针棒状、花瓣状,ZrC呈现规则的颗粒状;随着原始粉末中(Zr+B_4C)含量的增加,增强相ZrB_2和ZrC含量增多,尺寸变大,ZrB_2-ZrC/Fe涂层与Q235钢基体之间结合紧密,呈冶金结合;与Q235钢基体相比,ZrB_2-ZrC/Fe涂层耐磨性显著提高,最高可达基体的5.45倍,ZrB_2-ZrC/Fe涂层的磨损方式以磨粒磨损为主,断裂方式以穿晶断裂为主。     

Si3N4对碳/碳复合材料表面SiC涂层耐磨性的影响

为了提高碳/碳复合材料表面SiC涂层的耐磨性,采用包埋法和氮化处理制备SiC/Si₃N₄涂层。通过X射线衍射仪（XRD）、扫描电子显微镜（SEM）、能谱分析仪（EDS）及摩擦磨损试验,分别评价SiC涂层与SiC/Si₃N₄涂层的表面形貌、物相组成、磨损形貌及摩擦磨损性能,并研究涂层显微组织结构与磨损机理之间的联系。结果表明：SiC/Si₃N₄涂层由Si₃N₄相、SiC相和C相组成,涂层平整且致密;SiC/Si₃N₄涂层的摩擦系数低于0.05且更稳定;SiC涂层高摩擦系数值的主要磨损机制是黏着磨损和磨料磨损;SiC/Si₃N₄涂层中形成了一层较薄的润滑膜,并在摩擦磨损的后续阶段降低摩擦系数。Si₃N₄相的引入可以有效改善SiC涂层的表面结构,使得SiC涂层摩擦系数更小且更稳定,从而提高...     

Influence of Preparation Technology on the Structure and Phase Composition of MoSi2-Mo5Si3/SiC Multi-coating for Carbon/Carbon Composites

Oxidation protective MoSi₂-Mo₅Si₃/SiC multi-coatings for carbon/carbon composites were prepared by chemical vapor reaction and slurry-sintering method. The influence of preparation technology on the structure and phase composition of the coating was investigated by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD) analyses, and then their relationship was discussed. The results indicate that the Si/Mo ratio of the slurry and sintering processing were two main factors that significantly affected the structure and phase composition of the multi-coating. Appropriate sintering process and relatively high Si/Mo ratio were essential for preparing the multi-coating with dense structure and favorable phase composition. After being sintered at 1723 K for 2 h and with the Si/Mo ratio of the slurry being 4.5 (weight ratio), a dense structure accompanied by favorable phase composition of the coating can be obtained. When heat treated at 2373 K for 1 h, this coating became more compact and continuous. Oxidation tests (performed at 1623 and 1823 K) demonstrated that both of these two obtained multi-coatings exhibited better anti-oxidation property than single layer SiC coating.     

Cf/ZrC-ZrB2-SiC-C超高温陶瓷复合材料的显微结构表征

利用X-射线衍射、扫描电子显微镜和透射电子显微镜对Cf/ZrC-ZrB2-SiC-C超高温陶瓷复合材料的相组成、纤维/热解碳层的界面特征和超高温陶瓷基体的显微结构特征进行了表征。在碳纤维表面有一层厚度为2～3μm石墨化程度较高的热解碳界面层,该界面层可以避免采用PIP工艺制备超高温陶瓷基体时可能对碳纤维造成的损伤。热解碳层与碳纤维之间为弱机械结合,其界面间分布着20～30 nm的ZrC纳米颗粒。Cf/ZrC-ZrB2-SiC-C超高温陶瓷复合材料基体主要由ZrC,ZrB2,SiC和石墨相(Cg)组成。基体中石墨的(002)面沿着ZrC,ZrB2或SiC的表面生长。在石墨与ZrB2和石墨与SiC的界面没有观察到取向关系,界面处既没有反应层也没有非晶相存在。在石墨与ZrC之间存在ZrC(111)∥Cg(002),ZrC[110]∥Cg[010]的取向关系。ZrB2和SiC之间也没有界面反应和非晶层存在。     

Ablation characteristics of mosaic structure ZrC-SiC coatings on low-density,porous C/C composites

Mosaic structure Zr C-SiC coatings were fabricated on low-density, porous C/C composites via thermal evaporation and an in-situ method. Zr C was packed in a typical lamellar mode, and the mosaic structure was formed by the deposition of Zr and Si atoms on the shallow surface of the porous C/C composites.Ablation analysis showed that the defects in the coatings originate from the boundary between the Zr C and holes created by the consumption of SiC at 2500?C. After ablation for 200 s at 3000?C, a dense ZrO_2 layer formed on the coating surface, and the defects were sealed owing to the continuous supply of ablative components. The mass and line ablation rates of the Zr C-SiC coatings were-0.46 ± 0.15 mg cm~(-2)·s~(-1) and-1.00± 0.04 μm s~(-1), respectively.     

Mo5Si3-MoSi2/SiC复合涂层的高温抗氧化行为分析

采用化学气相反应法和料浆刷涂反应法,在石墨表面制备了Mo₅Si₃-MoSi₂/SiC复合涂层,借助X射线衍射仪、扫描电镜及能谱等分析手段,研究了涂层的结构;通过恒温抗氧化实验及热力学分析,重点研究了涂层的高温抗氧化行为。结果表明：在1823 K的氧化氛围中,复合涂层中的Mo₅Si₃、MoSi₂组元易氧化生成MoO₃气体并导致涂层失重;而氧化初期(0～6 h)涂层试样的增重则主要与SiC的惰性氧化主导有关。由于复合涂层各组元在高温下都能氧化生成SiO₂玻璃,使涂层具有良好的高温抗氧化及热震性能;经20 h、16次循环热震实验后,涂层试样的氧化失重率只有3.78%。     

Oxidation of ZrB<Subscript>2</Subscript> and its composites: a review

The oxidation behavior and oxidation mechanisms of monolithic ZrB₂ and particulate-ZrB₂ matrix composites were reviewed. Dispersion of SiC particles into ZrB₂ was found to be an effective way to prevent extensive oxidation. However, the formation of a SiC-depleted layer can become a critical problem because it can lead to spallation and delamination of the protective surface layer. The addition of ZrC in conjunction with rapid heating to temperatures higher than 2000 °C effectively reduced the porosity of the SiC-depleted layer. The formation of a dense surface layer was attributed to large volumetric expansion during the conversion from ZrC to ZrO₂. The effect of the ZrC addition depended on the temperature, heating rate, and composition. This review showed that material design for specific applications is required for high-temperature applications to maximize the oxidation resistance of ZSZ composites.     

SiC过渡层对SiC/Si-MOSi2涂层抗氧化性能的影响

采用液硅反应渗透和料浆烧结法在石墨表面制备SiC/Si-MoSi2抗氧化涂层.详细研究SiC过渡层对SiC/Si-MoSi2涂层抗氧化性能的影响.结果表明,SiC过渡层对SiC/Si-MoSi2涂层的抗氧化性能有很大影响,并从微观结构上分析和解释了SiC过渡层对所制备涂层抗氧化性能影响的原因.     

带有SiC浓度梯度炭材料的抗氧化涂层

在炭材料表面通过莫来石（３Ａｌ２Ｏ３·２ＳｉＯ２）或锆石（ＺｒＳｉＯ４）氧化物薄膜涂层与ＳｉＣ的浓度梯度薄层结合,成功地获得了在空气流中１４００℃下的高抗氧化性能。在１４５０℃时,采用将炭材料直接浸入熔融Ｓｉ金属形成ＳｉＣ浓度梯度,通过溶胶－凝胶过程形成锆石和莫来石氧化薄膜。水解速率的控制是产生均匀薄膜的关键。具有ＳｉＣ浓度梯度和莫来石涂层的各向同性高密度石墨块足以在空气中１４００℃下抗氧化和１４００℃到液氮温度下抗淬火。莫来石涂层比锆石涂层更有效。     

多孔氮化硅表面γ-Y_2Si_2O_7陶瓷涂层的制备及抗热震性能

采用浆料喷涂与高温熔渗结合的方法,以γ-Y_2Si_2O_7和Y_2O_3-Al_2O_3-SiO_2三元氧化物粉体为原料,在多孔Si_3N_4表面制备致密γ-Y_2Si_2O_7陶瓷涂层,采用XRD和SEM测试方法系统研究原料配比及烧结温度对涂层结构、组织和抗热震性能的影响。结果表明:SiO2与Al2O3物质的量之比较高时,涂层为致密γ-Y_2Si_2O_7层和过渡层的双层结构;SiO_2与Al_2O_3物质的量之比较低时,只能形成单层结构;双层结构涂层的抗热震性能优于单层结构涂层。     

W-Mo-Si/SiC Oxidation Protective Coating for Carbon/Carbon Composites

A W-Mo-Si/SiC double-layer oxidation protective coating for carbon/carbon （C/C） composites was prepared by a two-step pack cementation technique. XRD （X-ray diffraction） and SEM （scanning electron microscopy）results show that the coating obtained by the first step pack cementation was a thin inner buffer layer of SiC with some cracks and pores, and a new phase of （WxMo1-x）Si2 appeared after the second step pack cementation. Oxidation test shows that, after oxidation in air at 1773 K for 175 h and thermal cycling between 1773 K and room temperature for 18 times, the weight loss of the W-Mo-Si/SiC coated C/C composites was only 2.06%. The oxidation protective failure of the W-Mo-Si/SiC coating was attributed to the formation of some penetrable cracks in the coating.     

Effect of soft substrate on the indentation damage in silicon carbide deposited on graphite

Indentation-induced damage is investigated in silicon carbide (SiC) deposited on graphite substrate. The SiC films have been grown by LPCVD (Low Pressure Chemical Vapor Deposition) method using MTS (CH₃SiCl₃) as a source gas and H₂ as a diluent gas to provide highly dense deposited layer and strong interfacial bonding. The elastic-plastic mismatch is very high to induce distinctive damages in the coating and the substrate layer. The specimens with various coating thicknesses are prepared by changing CVD condition or mechanical polishing. Indentation damages with different sizes are introduced by controlling indentation load in Nanoindentation, Vickers indentation and Hertzian indentation test. Basic mechanical properties such as hardness, toughness, elastic modulus are evaluated against coating thickness. Mechanical properties are sensitive to the indentation load and coating thickness. The results indicate that coating thickness has a vital importance on the design of hard coating/soft substrate system because the soft substrate affects on the mechanical properties.