Si-Al-Ir Oxidation Resistant Coating for Carbon/Carbon Composites by Slurry Dipping

A Si-Al-Ir oxidation resistant coating was prepared for SiC coated carbon/carbon composites by slurry dipping. The phase composition, microstructure and oxidation resistance of the as-prepared Si-Al-Ir coating were studied by XRD (X-ray diffraction), SEM (scanning electron microscopy), and isothermal oxidation test at 1773 K in air, respectively. The surface of the as-prepared Si-Al-Ir coating was dense and the thickness was approximately 100 μm. Its anti-oxidation property was superior to that of the inner...     

K4104镍基高温合金Al-Si涂层高温氧化过程中的元素扩散分析

采用无机盐料浆法在K4104镍基高温合金表面制备Al-Si涂层。依据GB/T13303-91《钢的抗氧化性能测定方法》标准,采用静态增重法对有涂层试样和无涂层试样进行了1000℃×200h抗高温氧化性能试验,并绘制了氧化动力学曲线。用带能谱扫描电镜对氧化膜的表面形貌和截面组织进行分析,研究有无涂层试样在高温氧化过程中的元素扩散。结果表明:Al-Si涂层和基体合金之间在高温氧化过程中的互扩散形成了厚度为120~140um的渗层。随着氧化时间的延长,外层铝含量逐渐降低,但仍能保持稳定的β-NiAl相。Si在扩散作用下形成内高外低的分布形式,形成的Cr3Si和富Si的M6C相有利于阻止涂层和基体元素之间的互扩散,降低化合物层的形成速度,体现了Al-Si涂层良好的抗高温氧化能力。     

Oxidation Protective C/SiC/Si-SiC Multilayer Coating for Carbon/Carbon Composites Applying at 1873 K

A C/SiC/Si-SiC multilayer coating for protecting carbon/carbon(C/C) composites against oxidation was prepared by slurry and pack cementation.X-ray diffraction(XRD) and energy dispersive spectroscopy(EDS) analysis showed that the inner coating obtained from the slurry and pack cementation was a C/SiC gradient layer acting as bonding layer,and the exterior coating formed in the second pack cementation was a Si-SiC double phase coating.Oxidation tests at 1873 K in air showed that the coating exhibited excellen...     

高温氧化及热震对SiC/ZrB2-SiC/SiC涂层炭/炭复合材料力学行为的影响

为提高炭/炭(C/C)复合材料的高温抗氧化性能,同时分析涂层制备及高温氧化对涂层材料力学行为的影响,在C/C复合材料表面采用反应熔渗、料浆涂刷结合化学气相沉积工艺制备了SiC/ZrB2-SiC/SiC三层高温抗氧化涂层。利用SEM和XRD分析复合涂层的微观结构和相组成,考察涂层复合材料1500℃高温抗氧化和1500℃-室温的抗热震性能,研究高温氧化及热震对涂层C/C复合材料力学行为的影响。结果表明,复合涂层试样1500℃静态空气环境下具有优异的抗氧化及抗热震性能:1500℃氧化20 h后试样保持增重,1500℃至室温热震50次后增重为0.69%。因涂层制备过程中粉料的渗入反应,复合材料弯曲强度增长了7.08%。在经历1500℃氧化20 h和1500℃至室温50次热震后,涂层复合材料弯曲强度有所下降,且因材料界面结合力的减弱使得纤维拔出特征明显,材料塑性断裂特征增强。     

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.     

Oxidation Resistance of the Aluminide Coating Formed on Carbon Steels

Low and medium carbon steels were aluminized by the pack aluminizing technique using halideactivated pure-Al and Fe-Al packs. The effect of mixture composition, aluminizing temperatureand time and C content of the steel substrate on the structure and thickness of the aluminidelayer, and on the oxidation resistance was investigated. The optimum oxidation resistance canbe achieved with a low carbon steel substrate when the intermetallic phases Fe3Al and FeAlform the surface of the aluminide layer. In this case, the Al concentration at the surface of thealuminide coating is at least ≥15 wt pct. Formation of high Al concentration phases (FeAl3 andFe2Al5) during aluminizing should be avoided as they tend to embrittle the aluminide layer andreduce its oxidation resistance.     

Oxidation behavior and mechanical properties of C/SiC composites with Si-MoSi2 oxidation protection coating

A new kind of oxidation protection coating of Si-MoSi₂ was developed for three dimensional carbon fiber reinforced silicon carbide composites which could be serviced upto 1550 °C. The overall oxidation behavior could be divided into three stages: (i) 500 °C < T < 800 °C, the oxidation mechanism was considered to be controlled by the chemical reaction between carbon and oxygen; (ii) 800 °C < T < 1100 °C, the oxidation of the composite was controlled by the diffusion of oxygen through the micro-cracks, and; (iii) T > 1100 °C, the oxidation of SiC became significant and was controlled by oxygen diffusion through the SiC layer. Microstructural analysis revealed that the oxidation protection coating had a three-layer structure: the out layer is oxidation layer of silica glass, the media layer is Si + MoSi₂ layer, and the inside layer is SiC layer. The coated C/SiC composites exhibited excellent oxidation resistance and thermal shock resistance. After the composites annealed at 1550 °C for 50 h in air and 1550 °C 100 °C thermal shock for 50 times, the flexural strength was maintained by 85% and 80% respectively. The relationship between oxidation weight change and flexural strength revealed the criteria for protection coating was that the maximum point of oxidation weight gain was the failure starting point for oxidation protection coating.     

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.     

炭/炭复合材料表面C/SiC/Si-Mo-Cr多层复合防氧化涂层研究(英文)

为提高炭/炭(C/C)复合材料的高温抗氧化性能,采用料浆涂刷法首先在C/C复合材料表面制备了预炭层,然后以Si粉及石墨粉(Si粉与石墨粉的质量配比为:60～80:10～25)为原材料采用包埋法经高温热处理获得C/SiC内涂层,最后在涂有C/SiC内涂层的C/C复合材料表面采用包埋法制备Si-Mo-Cr外涂层。借助扫描电镜、X射线衍射、电子能谱等分析测试手段对涂层试样的微观结构进行了分析,研究了涂层C/C复合材料在1 873 K和1 973 K下的氧化行为。结果表明:由于涂层氧化过程中表面生成了SiO2和Cr2O3复合玻璃层,其在1 873 K温度下表现出优异的防氧化性能,可以有效保护C/C复合材料达135 h。当氧化温度提高至1 973 K并氧化30 h后,该复合涂层氧化过程玻璃层完整性被破坏,涂层失效。     

SiC-Si-ZrSiO_4 Multiphase Oxidation Protective Coating for Carbon/Carbon Composites

In order to improve the anti-oxidation property of carbon/carbon （C/C） composites, a novel SiC-Si-ZrSiO4 multiphase oxidation protective coating was produced on the surface of C/SiC coated carbon/carbon compo ites by a pack cementation technique. The phase composition and microstructure of the as-prepared coatings were characterized by XRD （X-ray diffraction）, SEM （scanning electron microscopy） and EDS （energy dispersive spectroscopy）. Oxidation behavior of the multiphase coated C/C composites was also investigated. It showed that the as-prepared coating characterized by excellent oxidation resistance and thermal shock re- sistance could effectively protect C/C composites from oxidation at 1773 K for 57 h in air and endure the thermal cycle between 1773 K and room temperature for 12 times, whereas the corresponding weight loss is only 1.47%. The excellent oxidation protective ability of the SiC-Si-ZrSiO4 coating could be attributed to the C/SiC gradient inner layer and the multiphase microstructure of the coating.     

水基浆料涂覆结合原位反应制备Cf/SiC复合材料表面光学涂层

本研究提出一种C_f/SiC复合材料表面改性新方法为水基浆料涂覆结合原位反应烧结工艺。系统研究了SiC和炭黑在水基浆料中的共分散、粘结剂的量和浆料固含量对浆料流变性能的影响、涂层的微观结构和性能等。研究结果表明: 采用水基浆料涂覆工艺可在基材表面制备一层气孔率达49%的多孔C/SiC预涂层; 通过液相渗硅原位反应工艺, 多孔预涂层转变为高致密、与基材强结合的光学涂层, 并且在涂层与基材间形成了~ 15 μm的化学反应过渡层; Si/SiC涂层的维氏硬度为(14.19 ± 0.46) GPa, 断裂韧性为(3.02 ± 0.30) MPa·m^1/2; 经过精细研磨抛光, 涂层的表面粗糙度可达2.97 nm RMS。     

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.     

碳/碳复合材料SiC/MoSi_2/ZrO_2涂层体系氧化烧蚀性能

抗氧化涂层技术是解决碳/碳复合材料高温抗氧化性的最有效技术途径之一。为了提高材料在1 800℃以上的高温抗氧化性能,首次采用包埋法、涂刷法和等离子喷涂法在碳/碳复合材料表面制备出SiC/MoSi_2/ZrO_2梯度抗氧化涂层体系。采用SEM/EDS、结合力和粗糙度测试对涂层表面及断面形貌进行微观分析,利用等离子风洞对整个涂层体系进行氧化试验。结果表明:基体、过渡层和高温抗氧化层之间结合力良好,高温抗氧化层厚度均匀、结构致密。经等离子风洞氧化600s后,涂层表面温度达到1 850℃,氧化质量失重速率仅为3.15×10~(-6) g/(cm~2·s)。表明SiC/MOSi_2/ZrO_2梯度抗氧化涂层体系在1 800℃以上的高温环境下具有很好的抗氧化性能。     

低密度碳粘接碳纤维复合材料(CBCF)抗氧化改性研究

以全氢聚硅氮烷(PHPS)为原料, 采用浸渍-热转化方法, 在低密度碳粘接碳纤维复合材料(CBCF)中短切碳纤维表面成功包覆硅氧氮(SiON)涂层。采用扫描电子显微镜(SEM)、能量色散X射线光谱(EDS)等分析测试手段对碳纤维表面的SiON涂层进行了形貌和物相分析, 结果表明: 涂层主要由Si、O、N元素组成, 在PHPS浓度为3wt%和5wt%条件下制备的涂层均匀、致密, 随着PHPS浓度的提高, 涂层厚度增加, 但易发生结块。当PHPS浓度为10wt%和20wt%时, 制备的SiON涂层出现结块并且存在裂纹。采用热重分析和等温氧化实验对纯CBCF和SiON涂层改性的CBCF复合材料抗氧化性能进行考核, 结果显示碳纤维表面包覆SiON涂层能够显著提高CBCF复合材料的抗氧化性, 随着PHPS浓度增大, 低密度CBCF复合材料抗氧化性能显著提高。     

MoSi2-SiC 抗氧化涂层对碳/碳复合材料弯曲性能的影响

在C/C 复合材料表面制备了MoSi₂-SiC 抗氧化涂层, 分析了涂层工艺对C/C 复合材料组织的影响, 测试了材料的室温弯曲力学性能。结果表明, 该工艺在C/C 复合材料表面生成抗氧化涂层的同时, 基材内部的层间和纤维束界面, 以及孔隙周围也被硅化。C/C 复合材料经涂层工艺处理后, 弯曲断裂行为发生改变, 弯曲强度明显升高,塑性有一定程度的降低。      

Al2O3对氩弧熔覆Fe-Si金属间化合物涂层组织及性能的影响

目前Fe-Si涂层的相关研究较少。为制备Fe-Si金属间化合物复合涂层并改善其力学性能,采用氮弧.熔覆原位合成的方法在Q235钢表面制备Fe-Si涂层和Fe-Si/Al2O3金属间化合物复合涂层,利用金相电子显微镜、X射线衍射仪(XRD)、冲蚀磨损试验机、高温氧化炉等设备对涂层的显微组织、耐冲蚀磨损性能和抗高温氧化性能进行测试与分析。结果表明:Fe-Si熔覆层由Fe3Si和FeSi相构成,添加A12O3后熔覆层除存在Fe3Si,FeSi外还有AI2O3相产生;Fe-Si/Al2O3熔覆层耐冲蚀磨损性优于Fe-Si熔覆层,最高为基体的4.65倍;熔覆层的耐高温氧化性能相对基体明显提高,在800℃下Fe-Si熔覆层和Fe-Si/Al2O3熔覆层相比于基体分别提高了5.50和5.83倍。     

Multi-composition oxidation resistant coating for SiC-coated carbon/carbon composites at high temperature

This work proposes a multi-composition oxidation resistant coating for SiC-coated carbon/carbon (C/C) composites by slurry method using the mixture of Y₂O₃, ZrO₂, Al₂O₃, Si and C. XRD analysis shows that the phases of the composite coating are composed of SiC, Al₂O₃, Y₂O₃, ZrO₂, Al₄SiC₄ and Y₃Al₂(AlO₄)₃. SEM analysis of the cross section of the coating displays the microstructure with 500 μm thickness which filled the porous SiC. Oxidation test shows that, after 19 h oxidation in air at 1873 K, the weight loss of the coated SiC-C/C is only 1.76%. The oxidation of the coated C/C composites was primarily due to the reaction of C/C matrix and oxygen diffusing through the penetrable cracks and bubble holes in the coating.     

磁控溅射TiAlSiN膜的抗氧化性能

目前,针对TiAlN和TiAlSiN薄膜在800~1 000℃高温氧化时的硬度及抗氧化性能研究较少。利用磁控溅射技术,在高速钢W18Cr4V表面制备了TiAlN和TiAlSiN薄膜,当Al靶功率为100 W、Si靶溅射电流为0.20 A时,TiAlSiN薄膜硬度及弹性模量达到最大值,对此条件下的膜层进行了大气高温氧化试验。采用激光共聚焦显微镜、扫描电子显微镜(SEM)和能谱仪(EDS)、X射线衍射仪(XRD)等检测手段,研究了800,900,1 000℃下2种薄膜的抗氧化性。结果表明:经相同温度氧化处理后,TiAlSiN薄膜的表面粗糙度明显小于TiAlN薄膜的;在TiAlN中引入Si元素形成Si3N4包裹TiN纳米晶的复合结构,抑制了膜层中裂纹的形成,使TiAlSiN薄膜在相同氧化温度下的抗氧化性能比TiAlN薄膜更加优异。     

Phase constitutions of MoSiN anti-oxidation multi-layer coatings on CC composites by fused slurry

To improve the oxidation resistance of MoSi fused slurry coating fabricated in vacuum, MoSiN multi-layer coatings were synthesized on C/C composites in nitrogen atmosphere by fused slurry using same Mo and Si element powders. The phase compositions and microstructures were characterized by X-ray diffractometry (XRD), optical microscopy (OM), scanning electron microscopy (SEM) with energy-dispersive spectroscopy (EDS). The results indicate that the MoSiN coating contains SiC inner layer and MoSi₂/Si main layer, which was similar with MoSi coating. Additionally, a thin outer layer with nano-filiform morphology has been found on the coating surface, which consists of SiC, Si₃N₄, AlN, Al₂O₃ and sialon phase. Oxidation experiments show that the MoSiN multi-layer coating exhibits excellent oxidation resistance at 1400 °C and anti-oxidizing potential ability at 1450 °C.     

炭/炭复合材料高温防氧化陶瓷涂层的研究新进展

陶瓷涂层技术是解决炭/炭(C/C)复合材料高温易氧化难题的有效手段。本文阐述了C/C复合材料的氧化过程与抗氧化途径,综述了近年来国内外C/C复合材料高温防氧化单相、多相镶嵌,梯度复合,晶须增韧以及多层复合等陶瓷涂层体系的最新研究进展,并就陶瓷涂层目前存在的问题以及下一步研究的重点提出了一些见解。