C/SiC复合材料轻型反射镜光学改性涂层技术研究进展

轻型反射镜在空间光学系统中发挥着非常关键的作用,现在已发展到第四代C/SiC复合材料.C/SiC反射镜通常采用坯体+涂层的结构形式来满足轻量化和高分辨率的双重要求.因此,在反射镜制备过程中,涂层制备技术已成为制备反射镜材料的关键技术之一.目前涂层制备技术主要有CVD-SiC涂层技术、浆料预涂层Si/SiC涂层技术等.文章介绍了第四代C/SiC反射镜光学改性涂层的设计、制备,并介绍了近些年国内外的研究进展.     

SiC基反射镜制备工艺研究进展

空间系统用的高性能轻质反射镜的研究和应用正逐年稳定发展,本文从几种卫星反射镜材料的性能和特性出发,得出SiC及其复合材料作为反射镜材料性能最佳的结论;通过比较各种工艺制备SiC基反射镜性能,结果显示:只有CVD SiC能够作为反射镜反射光学表面.本文重点详细介绍了SiC及其复合材料反射镜制备工艺及方法特点,并对其工艺发展前景进行了展望.     

反应浸渗法制备SiC/FeSix复合材料

研究了在SiC+C坯体中加入Fe粉,用熔融Si进行反应浸渗,以制备不合游离Si的SiC/FeSix复合材料.结果表明:用本实验方法通过调整坯体中Fe含量可以制得不合游离Si的SiC/FeSix复合材料,该材料在室温下的抗弯强度为(220±10)MPa.文中推导了Fe含量与第2相组成的理论模型,同时讨论了热处理工艺对烧结的影响.     

3D C/SiC复合材料的孔隙率与性能的关系

用浸债裂解法（PIP）和均效化学气相渗透法（ICVI）混合工艺制备了3DC／SiC复合材料,研究了3DC／SiC复合材料中基体含量。孔隙分布特征与复合材料性能的关系。结果表明,基体中CVI－SiC相对含量增加,开孔率增加,闭孔率减少,复合材料的弯曲强度和抗氧化性能提高。孔隙对复合材料性能的影响关系是由两种基体的特点、结构、致密化工艺及氧化机理决定的。     

炭/炭复合材料MoSi2/SiC抗氧化涂层的研究

采用包埋法制备C／C复合材料抗氧化MoSi2／SiC梯度涂层，同时对抗氧化涂层的形成、组织结构以及抗氧化性能与渗料的关系和抗氧化机理进行了研究。结果表明：采用包埋法制备的C／C复合材料抗氧化MoSi2／SiC梯度涂层致密，但有少量裂纹，涂层有良好的抗氧化效果。当Si与SiC保持一定的比例时，渗料中MoSi2的含量为50％时，涂层具有最好的抗氧化效果；当MoSi2与SiC保持一定的比例时，渗料中Si的含量为20％时，涂层具有最好的抗氧化效果。     

SiC反射镜表面改性研究进展

采用SiC陶瓷作反射镜是目前国际上的一个研究热点。但是SiC陶瓷用作反射镜时存在各种类型的缺点,必须对SiC反射镜表面进行改性。本文综述了各种表面改性方法、制备机理以及优缺点,最后展望了未来SiC反射镜的发展方向：即低成本化和大型化。     

基体改性对SiC/SiC复合材料高温抗氧化性能的影响

采用先驱体浸渍-裂解工艺结合三种基体改性方式制备了SiC/SiC复合材料,通过形貌分析和力学性能测试,分析了基体改性对Si C/SiC复合材料高温抗氧化性能的影响。研究表明,经1200℃静态空气氧化100h后,三种基体改性的复合材料弯曲强度几乎没有下降,氧化200h后,弯曲强度保留率均可达到80%;氧化300h后,复合材料内部结构没有氧化现象,表面区域界面层的氧化程度降低。改性基体中的B元素氧化生成液相封填SiC涂层表面,延缓了SiC涂层的氧化进程,并阻止氧化介质进入复合材料内部,保护纤维和界面层,从而使SiC/SiC复合材料的长时静态高温抗氧化性能明显提高。     

空间望远镜用C/SiC镜面研制综述

综述了空间望远镜的主镜用高强度、高表面精度、低热膨胀系数的低温（约4K）用镜面的制备和检测过程.日本将Φ710mm的高强度反应烧结SiC材料已用于红外望远镜镜面.在短切炭纤维增强C/C复合材料毛坯的基础上进行液相硅渗透（LSI）而制备的C/SiC复合材料在光学镜面方面具有更大的优势.通过提高C/C复合材料毛坯中沥青基炭纤维体积分数及控制硅化速度,可有效地提高LSI-C/SiC复合材料的机械性能和表面光学精度;通过不同规格的炭纤维的混杂化,可使C/SiC复合材料热膨胀系数的各向异性降低至小于4％的差异.SiC、Si-SiC浆料涂层处理可有效地提高表面精度至2 nm rms的极高要求.     

Ti3SiC2/Al2O3复合材料的制备与性能研究

以TiC／TiO2/Si／Al／Ti等为主要原料，采用热压法原位合成Ti2SiC2／Al2O3复合材料，分别探讨了Al掺入量和工艺制度对Ti3SiC2/Al2O3复合材料物相、显微结构以及性能的影响。结果表明：原位合成制备的Ti3SiC2/Al2O3复合材料与传统方法合成制备的纯Ti3SiC2材料相比，材料的硬度和致密度均有很大的提高。     

C/C多孔体的制备及其对C/C-SiC-Si复合材料的影响

C／C—SiC—Si材料是一种新型的复合材料。本文通过反应熔渗法将液态硅渗入C／C多孔体中得到致密的C／C—SiC—Si复合材料。重点研究了制备C／C多孔体的树脂浸渍裂解法，并测定了在不同浸渍次数下得到的不同的C／C多孔体的体积密度和气孔率，用扫描电镜观察了其形貌，讨论了不同的C／C多孔体对C／C—SiC—Si复合材料最终形貌的影响。     

Fabrication and characterization of biomorphic cellular C/SiC–ZrC composite ceramics from wood

Biomorphic cellular C/SiC–ZrC composite ceramics were fabricated from pine and oak wood precursors. Carbonaceous preforms were first prepared by wood pyrolysis and subsequently infiltrated with polyzirconobutanediol (PZC) and polycarbosilane (PCS) to form the composite ceramics. TGA/DTG and dilatometric analysis were used to study the pyrolysis of the wood precursor. XRD and SEM analyses were applied to characterize the microscopic properties of the resulting biomorphic cellular C/SiC–ZrC composite ceramics. Compared with oak, pine was preferable for preparation of cellular C/SiC–ZrC composite ceramics because of its unique microstructure. The SiC–ZrC phase distribution differed within the composite ceramics. In addition, the compression strengths of wood, charcoal, and cellular C/SiC–ZrC composite ceramics were measured in the axis direction. Results showed the improved compression strength of biomorphic cellular C/SiC–ZrC composite ceramics when the impregnation cycles were repeated.     

Pressure‐less joining of C/SiC and SiC/SiC by a MoSi2/Si composite

A MoSi₂/Si composite obtained in situ by reaction of silicon and molybdenum at 1450°C in Ar flow is proposed as pressure‐less joining material for C/SiC and SiC/SiC composites. A new “Mo‐wrap” technique was developed to form the joining material and to control silicon infiltration in porous composites. MoSi₂/Si composite joining material infiltration inside coated and uncoated C/SiC and SiC/SiC composites, as well as its microstructure and interfacial reactions were studied. Preliminary mechanical strength of joints was tested at room temperature and after aging at service temperatures, resulting in interlaminar failure of the composites in most cases.     

Ablation behavior of C/SiC with YSZ and ZrB2 coatings under high-energy laser irradiation

Carbon fiber-reinforced silicon carbide (C/SiC) composites are important candidates for laser protection materials. In this study, ablation mechanism of C/SiC coated with ZrO₂/Mo and ZrB₂–SiC/ZrO₂/Mo under laser irradiation was studied. ZrB₂–SiC multiphase ceramic and ZrO₂ ceramic were successfully coated on C/SiC composite by atmospheric plasma spraying technology with Mo as transition layer. Phase evolution and morphology of composite were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Moreover, ablation behavior of the composite was investigated by laser confocal microscopy. Results showed that ablation mechanism of C/SiC composite was controlled by phase transformation, thermal reaction, and thermal diffusion, with solid–liquid transition of ZrB₂ and ZrO₂ being dominant factor. Endothermic reaction and good thermal diffusivity of coatings were also important factors affecting ablation performance. Reflectivity effect of ZrO₂ coating was limited under high-energy laser irradiation. Compared with ZrO₂/Mo single-phase-monolayer coating, designed ZrB₂–SiC/ZrO₂/Mo coating showed better ablation performance, and breakdown time of C/SiC increased from 10 to 40 s. The depletion of liquid phase in molten pool was identified as an important factor responsible for rapid failure of C/SiC. The coating failed when the entire liquid phase was consumed within molten pool, followed by rapid damage of C/SiC substrate. Results of this study can provide theoretical guidance and research ideas for design and application of laser protective materials.     

Ti3SiC2陶瓷粉末的制备

新型层状陶瓷材料Ti3SiC2集金属和陶瓷的优良性能于一身,如良好的导电导热性、耐氧化、耐热震、高弹性模量、高断裂韧性等,在高温结构陶瓷、电刷和电极材料、可加工陶瓷材料、自润滑材料等领域有着广泛的应用前景。本文综合介绍了Ti3SiC2粉末制备的研究进展。此外,作者以Ti／Si／C／Al元素粉为原料,采用无压烧结的方法制备出纯度较高的Ti3SiC2陶瓷粉末,为Ti3SiC2基复合材料的发展开辟了一条新途径。     

Tensile properties of two-dimensional carbon fiber reinforced silicon carbide composites at temperatures up to 2300 °C

Carbon fiber reinforced silicon carbide (C/SiC) composites are of the few most promising materials for ultra-high-temperature structural applications. However, the existing studies are mainly conducted at room and moderate temperatures. In this work, the tensile properties of a two-dimensional plain-weave C/SiC composite are studied up to 2300 °C in inert atmosphere for the first time. The study shows that C/SiC composite firstly shows linear deformation behavior and then strong nonlinear characteristics at room temperature. The nonlinear deformation behavior rapidly reduces with temperature. The Young’s modulus increases up to 1000 °C and then decreases as temperature increases. The tensile strength increases up to 1000 °C firstly, followed by reduction to 1400 °C, then increases again to 1800 °C, and lastly decreases with increasing temperature. The failure mechanisms being responsible for the mechanical behavior are gained through macro and micro analysis. The results are useful for the applications of C/SiC composites in the thermal structure engineering.     

Improved dielectric and electromagnetic interference shielding properties of ferrocene-modified polycarbosilane derived SiC/C composite ceramics

In order to enhance the dielectric and electromagnetic interference shielding (EMI) properties, the SiC/C composite ceramics were fabricated by pyrolysis of ferrocene-modified polycarbosilane. The microstructure evolutions, dielectric properties, EMI and microwave absorption properties of SiC/C composite ceramics were investigated. The increases of both ferrocene contents and annealing temperatures led to the increases of crystallizations of SiC and carbons. Crystallized carbons including carbon nanowires, turbostratic carbons, onion-like carbons and graphene-like carbons were obtained in the materials. The carbon nanowires were longest when the 5 wt.% ferrocene-modified polycarbosilane was annealed at 1250 °C. These carbons played a more important role than SiC in the increases of dielectric and EMI properties. The average real and imaginary permittivities of materials increased from 4.4 and 0.7 to 38.9 and 39.6, respectively. The materials exhibited high total shielding effectiveness, high absorption shielding effectiveness and low reflection shielding effectiveness, which were 36.6, 30.1 and 6.5 dB, respectively.     

Preparation of SiC/C composite sheet from polycarbosilane/carbon-based resin mixture

SiC/C composites were prepared from a mixture of polycarbosilane and phenolic resin with weight ratio of 2/1 and 1/1 using PVB as a binder. The two types of green bodies which were formed by mould pressing method were treated in the temperature range from 1,000‡C to 1,500‡C under nitrogen. X-ray diffraction patterns, density, flexural strength and fracture surfaces of the composite were examined. The flexural strength of the composites at room temperature increased with heattreatment temperature and showed a maximum value of 175 MPa at 1,300‡C. When the composite was heat treated at 1,400‡C, the flexural strength decreased rapidly due to the crystallization of SiC. The SiC/C composites showed good oxidation resistance up to 830‡C. The effective mixing ratio of PCS/phenolic resin to obtain improved mechanical property was 2/1.     

多孔SiC陶瓷/石蜡复合相变材料定型封装及热性能研究

以微米级SiC粉为原料,采用冷冻干燥工艺制备具有连贯层状孔结构的SiC陶瓷。以多孔SiC陶瓷为基体,石蜡为相变芯材,通过真空浸渍法制备多孔SiC陶瓷/石蜡复合相变材料,研究了石蜡在层状多孔SiC陶瓷内的浸渗行为及复合材料的储热性能。结果表明,层片状多孔SiC陶瓷的显微形貌对石蜡的浸渗过程及储热性能有明显影响。当石蜡负载量为21.7%(质量分数)时,复合相变材料熔融温度为59.6 ℃,凝固温度为53.9 ℃,相变潜热为28.4 J/g,室温下的热导率为2.4 W·(m·K)^-1。复合相变材料吸热峰和放热峰强度随着石蜡负载量减少而降低,当温度为200 ℃时,多孔SiC陶瓷/石蜡复合相变材料失重为5%(质量分数),表明材料具有良好的热稳定性。复合相变材料在100 ℃热处理30 min后陶瓷基体未发生形变,经100次热循环后具有稳定的相变潜热和良好的定型能力。     

Effect of oxidation and residual stress on mechanical properties of SiC seal coated C/SiC composite

The effect of oxidation and thermal residual stress on mechanical properties of SiC seal coated C/SiC composite at ambient temperature and high temperature were studied. The oxidation of SiC seal coated C/SiC composite at 1300 and 1500 °C resulted in carbon fibres burn area near through thickness micro cracks in the SiC seal coating. With the increase in exposure time, the formation of SiO₂ layer in SiC matrix near carbon fibres burns area was found. Residual mechanical properties of SiC seal coated C/SiC composite after exposure in air show significant degradation. First time, a continuous measurement of Young's modulus with temperature of C/SiC composite was carried out using an impulse excitation technique. The effect of relaxation of thermal residual stress on mechanical properties was observed with the help of continuous measurement of Young's modulus as a function of temperature in an inert atmosphere.