等离子-物理气相沉积硅/莫来石/硅酸镱环境障涂层的高温防护和耐热冲击性能研究

通过SiCf/SiC复合材料表面等离子喷涂(APS)硅黏结层和莫来石中间层,等离子-物理气相沉积(PS-PVD)制备硅酸镱面层,喷涂的整个环境障涂层体系组织致密,PS-PVD工艺制备的硅酸镱为层状结构,孔隙率＜1％.研究了 SiCf/SiC复合材料环境障涂层的抗静态氧化、循环氧化、水汽腐蚀和热冲击性能,发现复合材料表面...     

盐雾腐蚀对热障涂层高温循环氧化性能的影响

利用电子束物理气相沉积法在Ni基高温合金表面制备了(ZrO₂＋MCrAlY)双层结构热障涂层。研究了常温盐雾腐蚀对其循环氧化行为的影响。试验结果表明涂层经过常温盐雾腐蚀后,陶瓷层的裂纹发生扩展,氧化锆晶体挤压、变形,同时由于常温盐雾环境的作用导致涂层在高温氧化过程中粘结层氧化严重,生成的热生长氧化层产生较大的体积膨胀效应,导致应力集中,降低了涂层的高温循环氧化性能,缩短了涂层的寿命。     

交流阻抗谱法评价热障涂层的热腐蚀行为(英文)

本文利用交流阻抗这种无损检测的方法研究了热障涂层在质量分数为25%NaCl+75%Na2SO4混合盐体系中的热腐蚀行为。实验结果显示,热腐蚀条件下,在陶瓷层和粘结层界面处形成TGO层为混合氧化物层,成分为Cr2O3、(Ni,Co)(Cr,Al)2O4和NiO,其厚度增长符合抛物线规律。热障涂层在110个循环腐蚀之前时,TGO层的电阻值随其厚度的增加而增加;110个循环后,虽然TGO层的厚度还是在增加,但由于TGO层孔隙的增多而导致其电阻值有所下降。陶瓷层的电阻值随着陶瓷层中裂纹的萌生和扩展而不断增大。等效电路中得到的参数可以用来表征热障涂层的失效行为。     

双层氧化物生长下热障涂层的界面失效与应力演化

在长时高温服役环境下,热障涂层（TBCs）会在内部的陶瓷层（TC）和粘结层（BC）之间生成由Al2O3层和混合性氧化物层（MO）组成的双层热生长氧化物（TGO）。其中,后期生成的MO 由于其疏松多孔、脆性大等特点,极易造成涂层内微裂纹的形成和扩展,导致涂层的过早剥落。因此,依据双层TGO 生长的扩散—氧化模型,在考虑材料非线性变形行为的基础上,运用生死单元法模拟TBCs 内双层TGO 异向生长下涂层界面的失效与应力演化过程。结果表明：MO 的生长会大幅度提升涂层界面的拉伸应力水平,易导致MO/TC 界面在高温阶段波峰区域和冷却阶段斜坡中心区域发生破坏及失效;MO/TC 界面的失效会引起BC 层波峰处更高的拉伸应力,促进冷却阶段Al2O3/BC 界面从波峰向波谷处的破坏;MO/TC 界面失效后,hAl2 O3 /hMO 的增加会加速Al2O3/BC 界面的破坏。     

等离子喷涂LaTi2Al9O19热障涂层的微观组织结构及热物理性能

 第一代热障涂层(TBCs)由氧化钇部分稳定的氧化锆(YSZ)陶瓷隔热层和金属粘结层组成,该涂层长期使用温度低于1 200℃。随着先进航空发动机向着高推重比发展,迫切要求发展新一代超高温、高隔热热障涂层材料。LaTi₂Al₉O₁₉(LTA)在1 500℃长期保持相稳定,是一种非常有前景的超高温热障涂层候选材料。本文采用大气等离子喷涂(APS)制备了LTA涂层,研究了喷涂工艺对涂层微观组织结构和热物理性能的影响。结果表明沉积态涂层中含少量的非晶态,在860℃和1 130℃出现晶化峰。等离子喷涂过程中La₂O₃挥发量较多,导致沉积态涂层中La元素与原始粉末相比含量偏低,而其他组分的化学成分随喷涂功率变化不大。LTA涂层的热扩散系数在1 400℃下为0.3~0.4 mm²·s^-1,热导率为1.1~1.6 W·m^-1·K^-1。1 050℃经过20小时热处理后,得到晶化的涂层在晶化温度范围内的热扩散系数和热导率值均增大。随着喷涂功率减小,涂层孔隙率增加,热导率减小。     

梯度热障涂层的设计

 采用电子束物理气相沉积方法 (EB PVD)制备了梯度热障涂层,其结构设计为NiCoCrAlY粘结层 /Al₂O₃ YSZ过渡层 /YSZ陶瓷层。YSZ陶瓷层的结构为柱状晶结构,Al₂O₃ YSZ梯度过渡层为梯度微孔结构。采用有限元方法对梯度热障涂层进行热应力分析,优化了Al₂O₃ YSZ梯度过渡层的组成。计算结果表明,梯度涂层的内应力显著降低,而且界面及其附近应力和应变变化较平缓。过渡层厚度的增加有利于降低涂层内应力和缓和涂层界面处的应力集中。     

Effect of boron doping on waterproof and dielectric properties of polyborosiloxane coating on SiO2f/SiO2 composites

A hydrophobic coating of the silica fiber reinforced silica composites (SiO_2f/SiO₂) was synthesized by sol-gel method using methyltriethoxy-silane (MTES) and boric acid (B(OH)₃) as raw materials. The relationship among boron doping, chemical structure of precursors and durability of hydrophobic coatings was discussed. The Si-O-B and methyl groups were successfully introduced in the gel precursors according to the FT-IR and XPS results. The resins were filled in the internal and surface holes of the SiO_2f/SiO₂ composites partially or completely, which is beneficial to reduce the physical adsorption of the moisture. In addition, hydroxyl groups of the SiO_2f/SiO₂ composites reacted with the resins and hydrophobic methyl groups were introduced, leading to the reduction of the chemical adsorption of water. Also, the boron doping was beneficial to enhancing the physical cross-linking between the coating and the SiO_2f/SiO₂ composites, and improved the adhesion of the coating to the substrate. The results show that the optimal hydrophobic coating with contact angle 130.33°, moisture absorption 0.33% and adhesion level 1 is obtained when the molar ratio of MTES to B(OH)₃ is 10:4. The real permittivity of M10B4 is constant in the range of 2.32–2.51 and the dielectric tangent loss is constant in the range of 5.5 × 10⁻⁴–8.7 × 10⁻³. The hydrophobic coating has excellent dielectric properties.     

不同制备工艺对MoSi2涂层抗氧化性能的影响

为解决MoSi2和SiC线膨胀系数差异,在带有SiC外涂层的C/C复合材料表面采用等离子喷涂、电弧沉积和固渗等工艺制备MoSi2涂层。涂层表面形貌分析发现,等离子喷涂MoSi2涂层多孔不致密,电弧沉积MoSi2涂层易开裂剥落;而固渗MoSi2涂层致密均匀,且界面结合力好。氧化试验也表明,固渗MoSi2涂层性能较好。     

Effects of Shot Peening Process on Thermal Cycling Lifetime of TBCs Prepared by EB-PVD

Conventional two-layered thermal barrier coatings (TBCs) are prepared by electron beam physical vapor deposition (EB-PVD) with ZrO2-8 wt% Y2O3 (8YSZ) as top coat and CoCrAlY as bond coat on disk-shaped Ni based super-alloy. In this paper, three kinds of shot peening process with different lengths of operating time were adopted for bond coating. As a result, changes took place in its sur- face roughness and the surface micro-hardness. A thermal cycling test at 1 273 K×55 min and another at room temperature for 5 min were performed to study the effects of shot peening process on the thermal cycling lifetime of TBCs. It is found that a moderate shot peening process will be able to prolong the life time. The oxidation dynamic of the as-processed TBCs basically accords with the para- bolic rule, and the oxidation test also attests to the spallation between YSZ and thermal growth oxide (TGO) responsible mainly for the failure of TBCs.     

High-entropy (La0.2Nd0.2Sm0.2Gd0.2Yb0.2)2(Zr0.75Ce0.25)2O7 thermal barrier coating material with significantly enhanced fracture toughness

Poor fracture toughness leads to premature failure of La₂(Zr_0.75Ce_0.25)₂O₇ (LCZ) thermal barrier coatings in an elevated temperature service environment. A novel coating material, namely (La_0.2Nd_0.2Sm_0.2Gd_0.2Yb_0.2)₂(Zr_0.75Ce_0.25)₂O₇ (LNSGY) based on the high-entropy concept, was successfully fabricated by solid-state sintering. The microstructure of LCZ and LNSGY was investigated by X-Ray Diffraction (XRD), Raman Spectrometer (RS), Transmission Electronic Microscopy (TEM) and Scanning Electron Microscopy (SEM). The fracture toughness of the LCZ and LNSGY ceramics was evaluated. The LNSGY has excellent high-temperature phase stability, and the grain size of LNSGY ceramic is smaller than that of LCZ ceramic at an elevated temperature due to the sluggish diffusion effect. Compared with LCZ (fracture toughness is (1.4 ± 0.1) MPa∙m^1/2), the fracture toughness of LNSGY is significantly enhanced (fracture toughness is (2.0 ± 0.3) MPa∙m^1/2). Therefore, the LNSGY can be a promising advanced thermal barrier coating material in the future.     

防止 C/C 复合材料氧化的 MoSi2/SiC 双相涂层系统的研究

 由固相扩散-浸渗处理制备了防止碳/碳复合材料氧化的MoSi2/SiC双相涂层。通过对涂层的结构、成份以及氧化机理的研究表明，MoSi2/SiC双相涂层由内层为β-SiC和外层为MoSi2/SiC双相层构成，具有优异的高温抗氧化性能。     

热障涂层中TGO的生长行为

采用等离子喷涂法在高温合金IC10上先后沉积粘结层为NiCrAlYSi,陶瓷层为Sc2O3-Y2O3-ZrO2的样品。样品在热循环炉中1100°恒温氧化,观察样品不同氧化时间的断面形貌,并绘制了样品的增重曲线,以此分析高温时TGO的生长过程。     

表面处理对热障涂层界面微结构的影响

采用真空电弧离子镀技术在单晶高温合金DD32上制备HY5金属粘结层,通过振动光饰、吹砂2种不同的表面处理方法改变粘结层表面状态,再在粘结层表面利用电子束物理气相沉积技术制备陶瓷层。研究了不同处理方法对粘结层表面状态的影响;测试了不同表面处理方法下制备的热障涂层的高温氧化性能并对比分析了它们的变化规律。此外,探讨了不同表面处理方法对界面元素成分及失效特征的影响。研究结果表明,通过表面处理可以去除粘结层表面较大的凸起,提高表面平整度,提高热障涂层抗氧化性能。与粗糙界面相比,光滑界面形成的TGO层均匀致密,Al含量高。经长时间的高温氧化后,粗糙界面的TGO层出现明显皱曲现象,陶瓷层开裂剥落。     

Effects of Hybrid Voltages on Oxide Formation on 6061 Al-alloys During Plasma Electrolytic Oxidation

Plasma electrolytic oxidation (PEO) is carried out on 6061 Al-alloys in a weak alkaline electrolyte containing NaOH, Na₂SiO₃ and NaCl. Centered on the correlation of composition and structure, analyses by means of X-ray diffration (XRD), scanning electron microscope (SEM) and energy dispersive spectrometry (EDS) are conducted on the specimens, which have been PEO-treated under hybrid voltages of different direct current (DC) values (140-280 V) with constant alternate current (AC) amplitude (200 V). Attention is paid to the composition, properties and growth mechanism of oxide layers formed with hybrid voltages. Moreover, the main effects of DC value are discussed. Ceramic layers with a double-layer structure which combines hard outer and soft inner layers are found to be consist of α-Al₂O₃, γ-Al₂O₃ and mullite. With the DC values increasing, the growth of the ceramic layers tends to have increasingly obvious three-stage feature.     

High-temperature oxidation behavior and analysis of impedance spectroscopy of 7YSZ thermal barrier coating prepared by plasma spray-physical vapor deposition

Quasi-columnar structure 7YSZ(yttria stabilized zirconia) thermal barrier coatings(TBCs) are prepared by plasma spray-physical vapor deposition(PS-PVD) onto pretreated and un-pretreated bond coating, respectively. An isothermal oxidation experiment of 7YSZ TBCs is carried out in the atmosphere of 950 °C in order to simulate the high-temperature oxidation process of engine blades. The isothermal oxidation process of 7YSZ thermal barrier coatings is investigated systematically by impedance spectroscopy. The electrochemical physical model and equivalent circuit of columnar 7YSZ coatings are established. Results show that the isothermal oxidation kinetic curve of columnar 7YSZ thermal barrier coatings appears to follow the parabolic law. A pretreatment of bond coating can reduce the growth rate of the thermally grown oxide(TGO) layer, restraining the initiation and propagation of microcracks between YSZ and TGO layers. The oxidation rate constants of 7YSZ coatings with pretreated and un-pretreated bond coating are 0.101×10~(-12) cm~2·s~(-1) and 0.115 × 10~(-13) cm~2 ·s~(-1), respectively. Impedance analysis shows that the content of oxygen vacancies decreases and the density increases after the TGO layer is oxidized for 150 h. In addition, shrinkage microcracks formed by sintering during the oxidation process is the main reason for an increase of the capacitance and a decrease of the resistance in the grain boundary of YSZ.     

热障涂层氧化行为研究进展

综述了国内外粘接层氧化行为的研究进展,介绍了粘接层氧化动力学,热生长氧化物( TGO) 组

成、结构和形成规律,以及亚稳态Al2O3 向稳态Al2O3 的转变规律,分析了MCrAlY 粘接层及基体合金中的各种

元素对TGO 形貌和成分的影响,指出了深入研究粘接层氧化行为的方法以及热障涂层性能的改善措施。

     

表面改性C/C复合材料与LAS玻璃陶瓷的连接

采用MgOAl₂O₃SiO₂(MAS)玻璃作为中间层,对SiCMoSi₂表面改性的C/C复合材料与Li₂CO₃Al₂O₃SiO₂(LAS)玻璃陶瓷进行热压连接。通过正交实验,研究了连接温度、连接压力和保温时间对试样连接强度的影响,确定最佳工艺参数为：1 200 ℃,20 MPa,15 min,所得到连接接头的最高剪切强度可达30 MPa。利用扫描电子显微镜（SEM）、能谱仪（EDS）和背散射电子像（BEI)对SiCMoSi₂涂层、连接界面的形貌以及组成进行了分析。研究结果表明,SiCMoSi₂涂层与基体结合紧密,Si,C元素在界面处呈梯度状分布,形成厚度约为15 μm的过渡层。MAS玻璃中的组分与LAS玻璃陶瓷和SiCMoSi₂涂层存在相互渗透现象,形成紧密的C/C(SiCMoSi₂)/MAS/LAS结构,界面间的结合良好。     

Joining of SiO2 ceramic and TC4 alloy by nanoparticles modified brazing filler metal

Nano-Al₂O₃ particles modified AgCuNi filler was adopted to braze the SiO₂ ceramic and TC4. The effects of filler size as well as the brazing temperature on the interfacial microstructure and mechanical property of the joints were investigated. Nanoscale filler reduced the phases dimension and promoted the homogeneous distribution of microstructure, obtaining a higher joint strength when compared to microscale filler. The increase of brazing temperature made the accelerating dissolution and diffusion of Ti, which promoted the increase of thickness of Ti₄O₇ + TiSi₂ layer adjacent to SiO₂ ceramic and diffusion layer zone nearby TC4 alloy. The hypoeutectic structure was produced in the brazing seam due to the high Ti content. The maximum shear strength of ∼40 MPa was obtained at 950 °C for 10 min.     

沉积温度对碳芯SiC 纤维微观结构的影响

以沥青基碳单丝为基体,一甲基三氯硅烷为碳化硅前驱体,使用通电加热的冷壁CVD工艺,温度在1 473～1 773 K,制备了碳芯SiC纤维.采用扫描电子显微镜和拉曼光谱对纤维的表面形貌及结构进行了表征,研究了沉积温度对其结构的影响.结果表明,SiC涂层为β-SiC晶型.沉积温度的升高引起了沉积速率的增加以及SiC涂层晶粒尺寸的长大.同时,导致碳芯中心区域发生结构重排,引起了该区域取向度的提高以及晶粒尺寸的减小.     

电弧离子镀Al扩散障结构及抗高温氧化性能研究

采用电弧离子镀技术(AIP)在HY3(NiCrAlYSi)涂层与镍基高温合金(K5合金)之间沉积一层Al薄膜经过马弗炉870℃加热1h形成Al2O3作为扩散障层,研究了Al2O3对HY3(NiCrAlYSi)涂层与基体的元素互扩散的阻碍作用和对涂层氧化动力曲线的影响。对于添加扩散障层前后的试样,进行循环抗氧化试验来评价其抗高温氧化性能,并用扫描电镜(SEM)分析氧化前后试样微观形貌和成分,用X-射线衍射仪分析涂层的相结构。试验结果表明:Al2O3有效阻止基体与涂层之间的元素互扩散,提高了HY3(NiCrAlYSi)涂层和K5合金的抗高温氧化性能。