先驱体转化法制备连续SiC(OAl)纤维

先驱体聚铝碳硅烷经熔融纺丝、空气预氧化处理、1300℃烧成制得连续的含有少量铝和较多氧的SiC(OAl)纤维,即KD-A纤维.通过元素分析、拉伸强度测试及SEM,AFM,HRTEM,XRD等分析对纤维进行了表征.结果表明:连续KD-A纤维是非晶型的含铝SiC纤维,直径为12 μm～14 μm,具有较高的抗拉伸强度(2.6 GPa)和弹性模量(210 GPa),其耐高温和抗氧化性能明显优于Nicalon纤维,达到了Hi-Nicalon纤维的水平.     

基于包混和复合添加工艺的多孔碳化硅陶瓷的制备和性能

采用包混工艺合成核-壳结构的硅-树脂先驱体粉体,引入Al2O3-SiO2-Y2O3复合添加剂,通过成型、炭化和烧结工艺制备多孔碳化硅陶瓷。分析多孔碳化硅陶瓷样品的物相、形貌、孔隙率、热导率、热膨胀系数和抗热震性能。结果表明：复合添加能够在较低的温度下制得多孔碳化硅陶瓷;陶瓷样品的晶粒较小,明显增强了多孔碳化硅陶瓷的导热性能;复合添加提高了碳化硅陶瓷的抗热震性能,添加Al2O3-SiO2-Y2O3并且在1650℃下烧结制备的多孔碳化硅陶瓷经过30次热震后的抗弯强度损失率为6.5%;陶瓷样品的孔壁更加光滑,孔分布更均匀;复合添加对多孔碳化硅陶瓷热膨胀系数的影响较小。     

微波烧结碳化硅的制备

以硅粉为硅源,乙炔炭黑为碳源,通过微波加热的方法制备碳化硅。研究反应物密实度和反应物粒度对产物碳化硅粒度和形貌的影响,利用SEM和TEM等手段观察碳化硅的形貌。结果表明:采用自由堆积的乙炔炭黑和硅粉为反应物时,硅粉、碳粉表面存在的氧与其发生反应生成的Si O和CO,再通过气-气反应生成Si C晶须,生成产物包括Si C颗粒和晶须。当反应物加压后,生成的Si O与Si和C反应生成Si C颗粒,产物中只包括Si C颗粒。乙炔炭黑和硅粉反应过程中Si C通过扩散机制生成,碳颗粒的粒度决定了生成的Si C的粒度。     

Electrochemical corrosion of silicon carbide ceramics

Recently, SiC‐based ceramics have been found to exhibit corrosion damage patterns, which can only be explained by electrochemical processes. Therefore, the current work focusses on the electrochemical test procedures to determine the corrosion behaviour of solid state sintered silicon carbide (SSiC) ceramics in acidic and alkaline media. The corrosion current densities have been determined from linear voltammetric scans. At anodic polarization potentials, electrochemically induced etching patterns were observed in alkaline solution. The formation of pores and crevices during electrochemical oxidation in acidic solution could be monitored by field emission scanning electron microscopy (FESEM) in addition to transmission electron microscopy (TEM). Impedance spectra measured after anodic polarization could be described by the assumption of a pore model equivalent circuit.     

Dielectric properties of doped silicon carbide powder by thermal diffusion

The doped SiC powders were prepared by the thermal diffusion process in nitrogen atmosphere at 2 000℃. Graphite film with holes was used as the protective mask, The dielectric properties of the prepared SiC powders at high frequencies were investigated. The complex permittivity of the undoped and doped SiC powders was measured within the microwave frequency range from 8.2 to 12.4 GHz. The XRD patterns show that before and after heat treatment no new phase appears in the samples of undoped and nitrogen-doped, however, in the aluminum-doped sample the AIN phase appears. At the same time the Raman spectra indicate that after doping the aluminum and nitrogen atoms affect the bond of silicon and carbon. The dielectric real part （ε） and imaginary part （ε＂） of the nitrogen-doped sample are higher than those of the other samples. The reason is that in the nitrogen-doped the N atom substitutes the C position of SiC crystal and induces more carriers and in the nitrogen and aluminum-doped the concentration of carriers and the effect of dielectric relaxation will decrease because of the aluminum and nitrogen contrary dopants.     

热解温度对聚碳硅烷转化SiC陶瓷结构及介电性能的影响(英文)

采用真空高温裂解聚碳硅烷法制备β-SiC陶瓷粉末,并对热解产物进行TGA/DSC、XRD和拉曼光谱表征。通过矩形波导法测量β-SiC陶瓷粉末与石蜡复合材料在8.2~18GHz下的复介电常数来研究其介电性能。结果表明:复介电常数的实部与虚部均随着热解温度的升高而增大。高温下产生的石墨碳引起的电子松弛极化及电导损耗是复介电常数的实部与虚部增大的主要原因。     

Aluminum doping and dielectric properties of silicon carbide by CVD

Cubic β-SiC coating was grown onto the graphite substrate by the normal pressure chemical vapor deposition using CH3SiCl3 （MTS） as a source precursor at 1 150 ℃. But the hexagonal Al4SiC4 phase was generated in the doped process with trimethylaluminium （TMA） as the dopant. Microstructure of the deposit coating as-prepared was characterized by scanning electron microscope （SEM）, which consists of spherical particles with a very dense facet structure. The real component of permittivity ε＇ and dielectric loss tang of the coatings undoped and doped by TMA were carried out by a vector network analyzer in the microwave frequency ranges from 8.2 GHz to 12.4 GHz. The results show that both of them have low values, and doped coating has lower ε＇ and tan δ than undoped one due to the existence of Al4SiC4 impurity phase, which indicates that the desired Al/SiC solid solution at 1 150 ℃ in a normal argon atmosphere is not produced.     

碳化硅材料在冰晶石熔液中的侵蚀行为

研究了气、冰晶石、铝液三相区介质在温度为900℃时对碳化硅材料的侵蚀行为。分别用光学显微镜和扫描电镜观察了试样在熔液区域的横截面以及试样与三相区的界面形貌。研究结果表明：碳化硅材料在熔融的冰晶石混合介质中表现出良好的抗腐蚀性能；铝液对碳化硅材料有侵蚀作用，而电解质、空气界面对碳化硅有较强的腐蚀行为。分析和探讨了各相介质对碳化硅材料的腐蚀机理以及腐蚀产物的相组成。     

连续SiC纤维表面铂涂层的制备及抗氧化性研究

采用金属有机化合物化学气相沉积法(MOCVD)在连续Si C纤维表面沉积了约0.8μm厚的Pt涂层,用扫描电镜对涂层的形貌进行观察,用EDS能谱和XRD对涂层的成分进行了分析,并对沉积涂层后的纤维在不同温度和时间下的抗氧化性能进行了测试。结果表明,制备得到的铂涂层光滑致密,与纤维结合牢固,有效弥补了纤维表面缺陷;对沉积涂层后的纤维进行力学表征和抗氧化测试,发现铂涂层不仅增加了Si C纤维的抗拉强度,而且经700～1400℃氧化1 h后纤维的抗氧化性能大幅提高。     

SiC颗粒表面Mo涂层的制备与分析

采用磁控溅射法在碳化硅(SiC)颗粒表面成功制备了金属钼(Mo)涂层,分析了Mo涂层的成分和形貌;为改善初始涂层成分和形貌,对镀Mo改性SiC复合粉体进行了不同工艺的结晶化热处理,重点研究了热处理对SiC颗粒表面Mo涂层形貌和成分的影响。结果表明,磁控溅射法能够在SiC颗粒表面沉积Mo涂层,随磁控溅射时间的延长,SiC颗粒表面Mo涂层的粗糙度增大,但磁控溅射后SiC颗粒表面Mo涂层为非晶态。热处理能够有效改善SiC颗粒表面Mo涂层的成分、形貌及结晶状态,在600~1200℃之间结晶化热处理过程中,随热处理温度升高,SiC颗粒表面Mo涂层形貌主要经历了以下4个阶段变化:Mo涂层初步致密化—Mo的结晶致密化—Mo涂层的聚集长大—Mo与SiC之间化学反应;相应的Mo原子的存在状态也经历了如下变化:非晶态Mo原子—晶态Mo原子—Mo_2C和MoSi_2。其中800~900℃之间为最佳热处理温度,此时Mo涂层致密均匀包覆完整。SiC表面连续均匀致密的Mo涂层,有利于改善SiC颗粒增强金属基复合材料中基体与增强体之间的界面结合并控制不利界面反应,有利于复合材料综合性能的提高,必将扩大SiC颗粒作为增强体的应用范围。     

High temperature oxidation of silicon carbide based materials

The process of high temperature oxidation of two silicon carbide based materials differing by methods of their production and properties has been studied up to 1500°C in air. The oxidation was performed under the isothermal conditions and at the programmed heat rate of 10° per minute. It was found that the oxidation resistance of the material was the function of the presence of extrinsic metals having close affinity for oxygen. It was also found that under heating up to 1500°C in air phase transitions occurred in the SiC surface layer.     

拓扑法计算硅/碳化硅材料的电阻率

用拓扑关系将硅 /碳化硅材料转化为具有 3个不同显微结构单元的整体 ,建立了等效电路 ,结合相关试验 ,计算了不同显微组织的硅 /碳化硅材料的电阻率。得到的理论计算结果与实验值的综合相对误差仅为3.9% ,分析比较了各相含量和分布形态对硅 /碳化硅材料整体电阻率的影响。结果表明 ,提高低电阻率硅的体积含量和其分布连续性 ,可降低材料的整体电阻率。该方法可用来预测要得到所需电阻率材料中应具有的硅含量和分布形态 ,为确定制备材料的显微结构设计提供指导。     

Formation of a chromium-carbide conversion coating on silicon carbide

The formation of a chromium-carbide conversion coating on SiC was achieved using the pack-cementation technique. The conversion coating is intended to improve the corrosion resistance of SiC and its derivatives, such as SiC-base continuous fibers and composites, by forming a protective Cr₂O₃ scale upon exposure to high-temperature corrosive environments. Different pack chemistry and processing parameters were evaluated in the laboratory. Results indicated that the coating morphologies and compositions achieved were significantly affected by variation of these processing factors. In this paper, the conversion coating obtained from one of the systems investigated is reported. The coating consists of a multilayered structure with each of the sublayers containing a high-Cr concentration. In addition, the coating surface is relatively dense and pore free compared to the underlying SiC substrate material. A dense and pore-free morphology is highly desirable for coating applications, especially on porous substrates. The multilayered coating structure consists of the following sublayers: Cr₂₃C₆/Cr₇C₃/Cr₇C₃+Cr₃Si/Cr₅Si₃C_x/SiC substrate.     

连续氮化硅纤维的氧化行为与高温影响研究

连续氮化硅陶瓷纤维是透波／承载一体化陶瓷基复合材料的关键原材料,也是制约复合材料耐高温性能与力学性能的关键因素。本文系统研究了国防科技大学研制的连续氮化硅纤维的抗氧化性能,分析了高温处理后纤维的组成结构与力学性能变化规律。结果表明：1000°C氧化1h后纤维强度高于原始纤维强度,主要是形成的玻璃相能减少和弥补纤维的表面缺陷。随着空气中处理温度提高,氧含量增加,纤维表面形成的SiO₂层逐渐变厚,纤维强度明显降低。纤维在1200°C氧化1h后强度保留率为63%,表明在此温度以下纤维有较好的服役性能。另一方面,氮化硅纤维在1450°C N₂中处理1h的强度保留率为57%,表现出良好的耐高温性能。纤维表面氧化对其在N₂下的耐高温性能具有不利影响,1000°C氧化的纤维在1450°C处理后丧失强度,1500℃处理后形成氮化硅结晶,失重明显增长,纤维内部也开始产生缺陷。     

Effect of annealing on mechanical properties of silicon carbide sintered with aluminum nitride and scandium oxide

Beta-SiC powder samples containing 1 wt.% α-SiC as a seed and 10 vol.% AlN-Sc₂O₃ as a sintering additive were hot-pressed at 1900 °C for 1 h and subsequently annealed at 2000 °C for 1 h, 3 h and 6 h. When the annealing time was increased, the microstructure changed from equiaxed to elongated grains, which resulted in a self-reinforced microstructure consisting of elongated grains (hexagonal platelet grains in 3-dimensions). The development of a self-reinforced microstructure resulted in significant improvement in toughness. However, the improved toughness was offset by a reduction in strength. The typical fracture toughness and strength of the ceramics annealed for 6 h were 7.3 MPa·m^1/2 and ∼500 MPa, respectively.     

Magnetic properties of vanadium-doped silicon carbide nanowires

This study reports the magnetic properties of vanadium (V) doped single crystalline silicon carbide nanowires. The first principle calculation indicated that the V-doped cubic SiC phase can exhibit half-metallic ferromagnetic properties that are essential for the realization of spintronic devices. Based on this calculation, V-doped SiC nanowires were fabricated in a chemical vapor deposition process. The single crystalline β-SiC nanowires, which are doped with ca. 4 at.% of V, had diameters of < 100 nm and a length of several μm. High-resolution transmission electron microscopy observations revealed vanadium carbide (VC) phases in the nanowires, even at this low concentration of dopants. Magnetic characterization implies that the nanowires are a mixture of the diamagnetic phase of VC and ferro- or paramagnetic phases of V-doped SiC. These results suggest that the doping of transition metal having high solubility to the SiC phase can lead to the realization of dilute magnetic semiconductor behavior at very low temperature.     

硅及硅合金对反应烧结SiC耐磨材料性能与结构的影响

本文首先分析了熔渗材料硅及硅合金的润湿性、流动性、烧失率的变化.结果表明:熔渗材料硅在1 430℃,硅铁合金在1 470℃时润湿角小(分别为0°和6°)、流动性大(分别为267%和198%)、烧失率小(均小于15%).同时分析了反应烧结SiC耐磨材料性能,并采用扫描电子显微镜、X射线衍射仪、EDS分别对其显微结构、主晶...     

Electrochemical corrosion of liquid phase sintered silicon carbide ceramics

Liquid‐phase sintered silicon carbide (LPS‐SiC) is silicon carbide ceramic which contains sintering additives forming a liquid phase during sintering. These additives segregate in the grain boundary phase during cooling. The usually used Al₂O₃ dissolves partially in the SiC‐grains and therefore changing the conductivity of the SiC (core rim structure). This study is focused on the electrochemical properties of LPS‐SiC with yttria and alumina as sintering additives. Electrochemical corrosion behaviour of LPS‐SiC has been determined by linear and cyclic voltammetry in acidic and alkaline solution. The effect of anodic oxidation on the material has been monitored by field emission scanning electron microscopy (FESEM) and energy dispersive X‐ray spectroscopy (EDX) as well as by atomic force microscopy (AFM). The core‐rim structure of the investigated materials plays a decisive role in the vulnerability towards corrosion. If oxidative attack was found to occur under anodic polarization, it happened preferentially in the rim region of the SiC‐grains, while the core of the SiC‐grains remained basically unaffected.     

Design and finite element analysis of lightmass silicon carbide primary mirror

Primary mirror is one of the key components in the space remote sensing system. To minimize the mass of the mirror without compromising its stiffness and decrease the deformation of the mirror surface at the different temperatures are the mainly two objects in the development of the primary mirror. Silicon carbide （SIC）, the most promising optical material, was used as the material of the primary mirror with triangle lightmass structure in a Cassegrain system. By using finite element method, the properties of the SiC mirror were compared with that of the traditional Be mirror and fused silica mirror. The results of static, dynamic and thermo-mechanical analysis indicate that the deformation of the mirror surface caused by temperature field is much bigger than that caused by gravity field. The SiC mirror has the best overall properties, and the SiC material is much suitable for the primary mirror.