Intelligent cooling structure design of "Z-pins like" silicon rods to enhance the ablation resistance of C/C-ZrC-SiC composites above 2500 °C

In order to improve the ablation resistance of C/C-ZrC-SiC composites by reducing the damage of the protective oxide layer, novel "Z-pins like" silicon rods, which were designed and fabricated by liquid phase sintering, were utilised as a dissipative agent. The microstructure evolution and thermal dissipation behaviour were investigated after ablating above 2500 °C for 300 s. After the "Z-pins like" silicon rods were implanted, the anti-ablative property of the C/C-ZrC-SiC composites was drastically improved by the dissipative thermal protection mechanism. The linear ablation rate of the "Z-pins like" silicon rod-reinforced C/C-ZrC-SiC composite was -0.28 μm/s, which is 112.72% lower than the unmodified composite. Additionally, the actual ablative temperature dropped approximately 357 °C, which enabled abundant SiO₂ to remain in the ablation centre. Furthermore, a dense SiO₂-rich oxide layer with a low oxygen diffusion coefficient is formed that covers the entire ablative surface.     

常压CVD法制备氮氧化硅薄膜沉积特性的研究

采用常压化学气相沉积方法(atmospheric pressure chemical vapor deposition,APCVD)制备了氮氧化硅(Si—O—N)薄膜,研究了影响其沉积速率和生长模式的因素。在φ(NH_3):φ(SiH_4)=20:1,基板温度为650℃的条件下,当混合气体流量小于720ml/min时,薄膜的形成主要受气体扩散过程控制;当混合气体流量大于720 ml/min时,则主要受表面气相反应过程控制;混合气体流量为720 ml/min的条件下,氮氧化硅薄膜的沉积过程主要受基板表面的气相反应过程控制,薄膜沉积厚度与沉积时间成线性关系,反应速率为常数1640 nm/min,表面活化能为283 kJ/mol。通过SEM分析发现:氮氧化硅薄膜的形成方式符合三维成核模型,即反应初期Si,N,O等原子在基板表面相遇结合在一起形成原子团,一定数量的原子团构成临界核;反应中期临界核长大为岛状结构,岛不断长大,岛与岛之间相互接合形成通道网络结构;反应后期,原子不断填补网络空洞,最后成为连续薄膜。     

激光诱导二甲基二乙氧基硅烷气相合成碳化硅超细粉

本工作首次采用有机硅试剂二甲基二乙氧基硅烷为反应物，进行了激光导气相反应，制备出平均粒径为４０ｎｍ的非晶ＳｉＣ粉末，粉末中Ｃ／Ｓｉ比随反应气流量的变化而变化。非晶ＳｉＣ粉末在１８７３Ｋ，氮气中退火１ｈ后转变为β－ＳｉＣ及α－ＳｉＣ，同时，粉末中部分氧杂质及自由碳脱出粉末。     

Surface Pretreatments of Silicon Nitride for CVD Diamond Deposition

The efficiency of different surface pretreatments (four standard chemical etchings and four diamond powder abrasive procedures) on silicon nitride (Si₃N₄) substrates for chemical vapor deposition (CVD) of diamond has been systematically investigated. Blank Si₃N₄ samples were polished with colloidal silica (∼0.25 μm). Diamond nucleation and growth runs were conducted in a microwave plasma chemical vapor deposition apparatus for 10 min and 6 h, respectively. Superior results concerning nucleation density ( N _d∼ 10¹⁰ cm⁻² after 10 min), film uniformity, and grain size (below 2 μm after 6 h) were obtained for the mechanically microflawed samples, revealing that chemical etchings (hot and cold strong acids, molten base or CF₄ plasma) are not crucial for good CVD diamond quality on Si₃N₄.     

Silicon Nitride Derived from an Organometallic Polymeric Precursor: Preparation and Characterization

Partially crystalline Si₃N₄, with nanosized crystals and a specific surface area greater than 200 m²/g, is obtained by pyrolysis of a commercially available vinylic polysilane in a stream of anhydrous NH₃ to 1000°C. This polymer does not contain N initially. Crystallization to high-purity α-Si₃N₄ proceeds with additional heating above 1400°C under N₂. The changes in crystallinity, powder morphology, infrared spectra, and elemental compositions, for samples annealed from 1000° to 1600°C under N₂, are consistent with an amorphous-to-crystalline transformation. Although macroscopic consolidation and local densification occur at 1400°C, volatilization and accompanying weight loss limit bulk densification. The effect of temperature on specific surface area is examined and related to the sintering process. These results are applicable to pyrolysis, decomposition, and crystallization studies of ceramics synthesized by polymeric precursor routes.     

氮化制度对Si-Al-Al2O3体系合成Sialon的影响

以SiC、α-Al2O3微粉、Si粉、Al粉为原料,在1450℃流动氮气中制备Sialon/SiC材料。研究了不同温度保温氮化对Sialon合成的影响。研究结果表明:有部分硅粉残余没有氮化;在1100℃保温氮化的氮化率高于在1150℃、1200℃保温氮化;1100℃保温氮化,残余Si量少、分布均匀,残余硅熔聚现象较轻,利于Sialon的合成。     

利用粉煤灰生产SiC陶瓷原料

利用粉煤灰部分或全部代替石英砂,配以适量的锯末,在高温炉中特定的烧成制度下,采用SiO2-C还原法将粉煤灰中的二氧化硅与锯末中的碳结合制取高性能的SiC陶瓷原料。利用正交实验对合成工艺中的合成温度、保温时间、碳过量数进行了设计和探索性实验,并对合成产物中的碳化硅的含量进行了测试。研究表明,在经催化剂(FeCl26H2O)浸泡12小时,加入2%矿化剂,在1380℃的合成温度下,保温时间2小时,碳过量10%的情况下,生成的SiC陶瓷原料中SiC的含量在53.6%以上。     

Sol-Gel Alumina Coating for Improved Cyclic Oxidation Resistance of Silicon Nitride

A 25 nm thick α-alumina layer was deposited on a turbine-grade silicon nitride by sol-gel dip coating and subsequent heat treatment in air at 1200°C. This layer had a nanometer grain structure. Silicon nitride protected by this thin layer showed a significant improvement in oxidation resistance over its uncoated counterpart after 200 cyclic exposures in air at 1250°C. The oxide layer grown on the coated silicon nitride also exhibited superior surface morphology, compared with the uncoated silicon nitride.     

Microstructure and Mechanical Properties of Hot-Pressed Silicon Carbide-Aluminum Nitride Compositions

A flexural strength of up to 1 GPa was achieved in SiC-AIN materials and is attributed to a dense, equiaxial grain structure of the 2H(δ) SiC-AIN solid solution, with a relatively uniform grain size of ∼ 1 μm. The strength was found to decrease with increasing grain size. While the β→α phase transformation and the formation of various metastable polytypes make microstructural control difficult in SiC materials, excellent control is facilitated in SiC-AIN materials as a result of the stable 2H solid solution. Several mechanisms of grain refinement during the β→ 2H transition were observed, most notably the direct formation of several 2H grains from a single β grain. In addition, grain growth is limited by the diffusion-controlled nature of the transition. These mechanisms could be utilized to achieve even higher strength values, with potentially higher reliability of the materials in structural applications.     

Molybdenum Oxycarbide and Tungsten Oxycarbide Coatings on Silicon Carbide Fibers

The strength and toughness of fibrous composites depend on the interface properties which control the bonding between the fibers and matrices. One method of controlling the interface involves coating the fiber with an appropriate material. In a previous study, it was found that there is a definite advantage in using low coating temperatures to prevent fibers from degrading. We therefore were interested in a report that Mo₂C could be deposited from Mo(CO)₆ at temperatures as low as 300° to 475°C. Our studies indicated that the material was not Mo₂C, but an oxycarbide, which, with an analogous tungsten oxycarbide coating, was applied to SiC yarns. Both oxycarbides could be converted to the metals by heat-treating in N₂.