炭/炭复合材料高温抗氧化MoSi2/SiC复合涂层及其抗氧化特性

采用两段式包埋法和封闭处理的复合新工艺制得抗氧化性优良的MoSi₂/SiC复合梯度C/C复合材料高温抗氧化涂层。涂层由内至外结构为:SiC过渡层→SiC致密层→MoSi₂/SiC双相层→以MoSi₂为主的外层。对未封闭处理的涂层,制备过程中高温保温时间长的氧化失重少,1200℃、1300℃空气中氧化失重比1400℃、1500℃氧化失重大。用正硅酸四乙酯对涂层表面进行封闭处理,凝胶形成的SiO₂可充填涂层表面裂纹并覆盖在涂层表面。在1500℃空气中氧化一定时间后,未封闭处理的涂层试样表现为氧化失重;封闭处理后的试样为氧化增重,氧化52h仍然只有1.28%的增重,封闭处理使涂层的抗氧化性能明显改善。      

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。     

炭/炭复合材料SiC/SiC+mullite/mullite涂层制备及其高温性能

为提高炭/炭复合材料的防氧化性能,采用包埋法与超音速等离子喷涂法相结合,在其表面制备了SiC/SiC+mullite/mullite多层防氧化涂层.外涂层主要组成是莫来石(mullite)相.对涂层试样进行了1 500℃恒温氧化和1 500℃～室温热震测试.实验结果表明,涂层试样经1 500℃恒温氧化150 h后,失重率仅为0.26%;经1 500℃～室温15次热震后,失重率仅为0.25%,显示出较优异的防氧化、抗热震性能.莫来石(mullite)具有良好的耐高温性能、低的氧扩散率,且SiC涂层氧化生成的SiO2在高温下能够愈合裂纹等缺陷,这是SiC/SiC+mullite/mullite涂层较好防氧化能力的主要原因.     

炭/炭复合材料自愈合涂层的制备及其抗氧化性能

为了拓展C/C复合材料作为高温结构材料的应用领域,作者研究制备了一种具有自愈合功能的 C/C复合材料抗氧化涂层,它主要由SiC和Si-B-Al-Cr-Zr系陶瓷氧化物构成.静态干燥空气中的氧化试验显示,对应700～1 000 ℃的平均氧化失重率约为2.91×10-7～9.43×10-6 g/(cm2·s);涂层在1 000 ℃以内温度环境下具有良好的抗氧化能力;5～6个300～1 000 ℃热循环内涂层试样氧化速率下降,其后增加,6 h内经过10次300～1 000 ℃热循环后涂层试样氧化失重为19.64%,涂层在一定热循环范围内具有抗热震性能.SiC结合B基陶瓷为主要组分的涂层能够在较长氧化时间和一定的热震循环周期内保持涂层试样较低的氧化失重率并降低其氧化速率.     

C/C复合材料SiC/ZrB_2-MoSi_2复合涂层的抗氧化机制

采用包埋法和刷涂法在C/C复合材料基体上制备SiC/ZrB2-MoSi2抗氧化涂层,并利用SEM和XRD等测试手段对抗氧化涂层的组织结构、抗氧化性能和抗氧化机制进行了研究。研究结果表明,SiC内涂层可有效解决外涂层ZrB2-MoSi2与C/C复合材料基体间热膨胀系数差异较大的难题。刷涂法制备的ZrB2-MoSi2外涂层虽然有大量的龟裂纹,但涂层试样在1500℃空气中氧化10 h,失重率仅为3.58%,涂层具有很好的自愈合能力,表现出优异的高温抗氧化性能和抗热震性能。     

航空刹车用自愈合抗氧化涂层的制备及性能

制备了一种具有自愈合功能的C/C复合材料抗氧化涂层,它主要由SiC和B4C、高熔点还原性氧化物等陶瓷细粉经简单工艺涂刷制成.通过动态氧气氛中的TGA试验、静态干燥空气中的氧化失重试验及扫描电镜、X射线衍射分析研究了其抗氧化和抗热震性能,试验结果显示,该涂层能承受1000℃以下40ml/min氧流量的动态氧化冲击;对应600～1000℃的静态氧化的平均氧化失重率介于10-8～10-6 g/(cm2·s)量级,涂层在1000℃以内的工作温度环境下具有良好的抗氧化能力;涂层试样经过10次热震循环后总的氧化失重为17.8%,在一定热循环范围内具有较好的抗热震性能;涂层试样的氧化失重率与氧化时间及热震次数具有非线性关系,表明该涂层具有自我愈合裂纹的功能.     

Cf/SiC复合材料SiC/(ZrB2-SiC/SiC)4涂层的制备及性能研究

以C_f/SiC复合材料为基体, 采用浆料浸涂法和脉冲CVD法制备了SiC/(ZrB₂-SiC/SiC)₄涂层, 借助XRD、扫描电镜及能谱对涂层的结构及组成进行了分析研究, 并初步考查了其高温抗氧化性能. 结果表明, 涂层总厚度约100μm, 主要由ZrB₂-SiC涂层与脉冲CVD SiC涂层交替覆盖而成. 在1500℃空气中氧化25h, 未涂层试样失重明显; 脉冲CVD SiC涂层试样氧化失重率为5.1%; 而SiC/(ZrB₂-SiC/SiC)₄涂层试样出现增重现象, 增重率达2.5%, 表现出优异的抗氧化性能.     

SiC/MoSi2-Si-Cr-B/玻璃涂层碳/碳复合材料抗氧化行为研究

采用两步包埋法及料浆涂刷-烧结法在二维碳布叠层碳/碳复合材料表面依次制备了SiC/MoSi2-Si-Cr-B包埋涂层及磷酸盐玻璃外涂层,研究了其在950℃静态空气环境中自由状态的抗热震、防氧化性能及不同弯曲变形状态下的防氧化性能,并借助X射线衍射分析仪及扫描电子显微镜对涂层试样的组成成分及微观组织形貌进行了分析.结果表明:950℃自由状态下该涂层体系的氧化失重率为负值,抗热震、防氧化效果良好;磷酸盐玻璃层在950℃软化熔融呈粘流态,可填补涂层内的裂纹和孔洞,阻止氧的入侵,有效提高了涂层整体的抗热震及抗氧化性能;但弯曲变形状态下,涂层试样的氧化失重率随形变量的增加而提高,形变会在一定程度上降低碳/碳复合材料抗氧化涂层的保护效果,加速材料的氧化失效.     

SiC-MoSi2涂层C/C复合材料的动态氧化行为研究

C/C复合材料在使用过程中往往经受急冷急热与高温燃气冲刷。为了研究涂层C/C复合材料的动态氧化行为及失效机制,本文对SiC/MoSi_2涂层C/C复合材料试样的全温抗氧化性能以及抗冲刷性能进行测试分析.结果表明:SiC/MoSi_2涂层试样具有良好的高温抗燃气氧化冲刷性能,在经历1 600℃高温燃气冲刷55.5 h,10次室温～1 600℃～室温急冷急热考核后,失重率仅为7.68%;涂层试样在高温风洞中动态氧化失效的原因是位于缺陷氧化最敏感温度处的试样微区的氧化损耗最为严重,导致试样在该微区处的力学性能显著下降,使其无法承受气动载荷而发生断裂.     

Cf/SiC复合材料SiC/(ZrB2-SiC/SiC)4涂层的制备及性能研究

以C_f/SiC复合材料为基体, 采用浆料浸涂法和脉冲CVD法制备了SiC/(ZrB₂-SiC/SiC)₄涂层, 借助XRD、扫描电镜及能谱对涂层的结构及组成进行了分析研究, 并初步考查了其高温抗氧化性能. 结果表明, 涂层总厚度约100μm, 主要由ZrB₂-SiC涂层与脉冲CVD SiC涂层交替覆盖而成. 在1500℃空气中氧化25h, 未涂层试样失重明显; 脉冲CVD SiC涂层试样氧化失重率为5.1%; 而SiC/(ZrB₂-SiC/SiC)₄涂层试样出现增重现象, 增重率达2.5%, 表现出优异的抗氧化性能.     

An approach to the mechanical behaviour of SiC/SiC and C/SiC ceramic matrix composites

The mechanical behaviour of two woven composites C/SiC and SiC/SiC was investigated at room temperature. The non-linear load-displacement curves and the damaging process were closely related to the specific structure of the composites, consisting of a network of impregnated bundles of fibres. The damage in the bundles proceeded by multiple cracking in the matrix before fibre failure, and dictated the response to the applied load. Other mechanisms, consisting mainly of distortions in bundles and their framework, induced a residual deformation and an energy dissipation. The behaviour was characterized according to the damaging process. Stress-electric strain curves revealed a mechanical response similar to those observed in unidirectional composites, although some effect of the specimen geometry on the curves was observed. Residual strains were similar in tensile and bending conditions. The work of fracture was consistently described by a volumetric rate of energy absorption, related to the applied strain, but the respective contributions of different damage mechanisms could not be determined.     

Phase formation and diffusion path of SiC/Ta/SiC joint

Abstracts are not published in this journal This revised version was published online in November 2006 with corrections to the Cover Date.     

Fatigue behaviour of 3-d SiC/SiC Composites

A tension–tension fatigue damage analysis was performed using 3-d silicon carbide fibre reinforced (orthogonal) silicon carbide matrix (SiC/SiC) composites. Two groups of SiC/SiC specimens were tested. The first group consisted of samples without any oxidation protective top layer coating, whilst the latter one contained samples covered with a well fitting, chemical vapour deposited (CVD) SiC system. This coating is necessary for the material to sustain high temperatures. Both the coated and uncoated material had a fibre volume fraction of about 36% equally distributed in three rectangular directions. Load control fatigue tests were conducted at room temperature. The fatigue life was found to decrease by increasing the cyclic stress level. A power-law equation is proposed, which correlates the applied maximum stress during the fatigue test with the number of cycles to failure. In general, the presence of the coating layer decreases the static strength of the material. However, the nominal maximum cyclic stress for which the endurance fatigue limit appeared, remained unaffected by the presence of the oxidation protective SiC coating. Microstructural examination has also been performed on the fractured specimens and it reveals some of the failure mechanisms of the composite that appeared under quasi-static and dynamic loading.     

C/SiC陶瓷基复合材料表面Si/SiC涂层制备

采用新的泥浆预涂层-反应烧结工艺在C/SiC复合材料表面制备Si/SiC致密涂层,重点研究了原材料、工艺条件对涂层性能的影响;采用XRD分析涂层的组分及晶体结构,采用SEM分析涂层的断口形貌.结果显示,采用MC为胶粘剂、较低的裂解升温速度制备的预涂层性能最好;无Si气氛存在直接高温烧结制备涂层性能差,而在真空环境下、1450～1600℃温度范围高温烧结能够制备出致密的Si/SiC涂层,Si气氛的大量存在是决定涂层性能的关键.     

Comparison of Fatigue Life Between C/SiC and SiC/SiC Ceramic-Matrix Composites at Room and Elevated Temperatures

In this paper, the comparison of fatigue life between C/SiC and SiC/SiC ceramic-matrix composites (CMCs) at room and elevated temperatures has been investigated. An effective coefficient of the fiber volume fraction along the loading direction (ECFL) was introduced to describe the fiber architecture of preforms. Under cyclic fatigue loading, the fibers broken fraction was determined by combining the interface wear model and fibers statistical failure model at room temperature, and interface/fibers oxidation model, interface wear model and fibers statistical failure model at elevated temperatures in the oxidative environments. When the broken fibers fraction approaches to the critical value, the composites fatigue fracture. The fatigue life S–N curves and fatigue limits of cross-ply, 2D and 3D C/SiC and SiC/SiC composites at room temperature, 550 °C in air, 750 °C in dry and humid condition, 800 °C in air, 1000 °C in argon and air, 1100 °C, 1300 °C and 1500 °C in vacuum, have been predicted. At room temperature, the fatigue limit of 2D C/SiC composite with ECFL of 20 % lies between 0.78 and 0.8 tensile strength; and the fatigue limit of 2D SiC/SiC composite with ECFL of 20 % lies between 0.75 and 0.85 tensile strength. The fatigue limit of 2D C/SiC composite increases to 0.83 tensile strength with ECFL increasing from 20 to 22.5 %, and the fatigue limit of 3D C/SiC composite is 0.85 tensile strength with ECFL of 37 %. The fatigue performance of 2D SiC/SiC composite is better than that of 2D C/SiC composite at elevated temperatures in oxidative environment.     

Modeling of electromechanical behavior of woven SiC/SiC composites

A coupled electro-mechanical model was developed to predict the mechanical behavior of woven SiC/SiC ceramic matrix composites and electrical resistance response to mechanical damages in the composites. The matrix is explicitly included in the model such that the matrix cracking and fiber break can be linked to the electrical resistance change during loading. The results show that the electrical resistance increases linearly with an increase of matrix crack density and the number of fiber breaks. The predictions are compared to the experimental results on 2D woven SiC/SiC ceramic composites. With proper materials parameters input, the models can accurately predict the stress–strain curve and electrical resistance change during the loading. The model is further compared to an analytical solution of electromechanical coupling to get an insight into the electrical–mechanical interaction mechanisms in the composites.     

不同界面SiC/SiC复合材料的断裂行为研究

碳化硅纤维增强碳化硅复合材料(SiC/SiC)是极具前景的高温结构材料。通过先驱体浸渍裂解(PIP)工艺分别制备了PyC界面和CNTs界面SiC/SiC复合材料, 对两种SiC/SiC复合材料的整体力学性能以及界面剪切强度等进行了测试表征, 并对材料中裂纹的产生与扩展进行了原位观测。结果表明, 两种界面SiC/SiC复合材料弯曲强度相近, 但PyC界面SiC/SiC复合材料的断裂韧性约为CNTs界面SiC/SiC复合材料的两倍。在PyC界面SiC/SiC复合材料中, 裂纹沿纤维-基体界面扩展, PyC涂层能够偏转或阻止裂纹, 材料呈现伪塑性断裂特征; 而在CNTs界面SiC/SiC复合材料中, 裂纹在扩展路径上遇到界面并不偏转, 初始裂纹最终发展为主裂纹, 材料呈现脆性断裂模式。     

Localized mechanical property assessment of SiC/SiC composite materials

SiC fiber-reinforced SiC matrix composites (SiC/SiC) are under consideration as a structural material for a range of nuclear applications. While these materials have been studied for decades, recently new small scale materials testing techniques have emerged which can be used to characterize SiC/SiC materials from a new perspective. In this work cross section nanoindentation was performed on SiC/SiC composites revealing that both the hardness and Young’s modulus was substantially lower in the fiber compared to the matrix despite both being SiC. Using scanning electron microscopy it was observed that the grain growth of the matrix during formation was radially out from the fiber with a changing grain structure as a function of radius from the fiber center. Focused ion beam machining was used to manufacture micro-cantilever samples and evaluate the fracture toughness and fracture strength in the matrix as a function of grain orientation in the matrix. Additionally microstructural characterization techniques like Raman spectroscopy, X-ray diffraction, and microtomography were used to evaluate differences in the matrix and fibers of the composite.     

SiC晶须增强SiCf/SiC复合材料的力学性能

以连续SiC纤维为增强体,采用前驱体浸渍裂解工艺,在复合材料基体中引入SiC晶须制备出多级增强的SiCf/SiC-SiCw复合材料,并采用化学气相渗透工艺在SiC晶须表面制备BN界面层,研究了SiC晶须及其表面BN界面层对复合材料的性能影响.结果表明:在复合材料中引入SiC晶须后,由于晶须的拔出、桥连及裂纹偏转等作用增加了裂纹在基体中传递时的能量消耗,使SiCf/SiC复合材料的压缩强度有明显提高,当引入体积分数为20％的SiC晶须时,复合材料压缩强度提高了22.6％,可达673.9 MPa.通过化学气相渗透工艺在SiC晶须表面制备BN界面层后,复合材料的拉伸强度、弯曲强度和断裂韧度分别为414.0,800.3 MPa和22.2 MPa·m1/2,较SiC晶须表面无界面层时分别提高了13.9％,8.8％和19.0％.