碳化硅质焊料连接氮化硅/碳化硅陶瓷的性能研究

采用以碳化硅为主相的焊料,在无压的条件下,连接氮化硅结合碳化硅陶瓷.结果表明:焊料在室温到1323K的干燥和烧结过程中,体积稳定,稍有膨胀.在1173K保温3h的条件下,连接的样品拉伸强度达到1.76MPa,热震残余强度保持率为82%.接头致密,并且焊料层与母材显微结构非常相似,界面处有明显的元素扩散,这对于提高结合强度和热震性能有重要作用.     

反应烧结制备Si3N4/SiC复相陶瓷及其力学性能研究

以两种不同配比Y₂O₃/Al₂O₃ (A, 2:3; B, 3:1, 总量15 wt%)为烧结助剂, 通过添加不同质量分数的SiC粉体,反应烧结制备了高强度的氮化硅/碳化硅复相陶瓷。并对材料的相组成、相对密度、显微结构和力学性能进行了分析。结果表明: 在1700℃保温2 h情况下, 烧结助剂A 与B对应的样品中α-Si₃N₄相全部转化为β-Si₃N₄; 添加5wt% SiC, 烧结助剂A对应样品的相对密度达到最大值94.8%, 且抗弯强度为521.8 MPa, 相对于不添加SiC样品的抗弯强度(338.7 MPa)提高了约54.1%。SiC能有效改善氮化硅基陶瓷力学性能, 且Si₃N₄/SiC复相陶瓷断裂以沿晶断裂方式为主。     

Si3N4／SiC纳米复合陶瓷的微观结构

利用ＪＥＭ２０００ＥＸⅡ高分辨电镜和ＨＦ２０００冷场发射枪透射电镜对Ｓｉ３Ｎ４ＳｉＣ纳米笔合陶瓷材料的微观组织，结构和成分进行了研究。结果表明，ＳｉＣ颗粒弥散分布基体相β－Ｓｉ３Ｎ４晶内和晶界，晶内ＳｉＣ颗粒与基体相的界面结构有三种类型；１）直接结合的的界面；２）完全非晶态的界面；３）混合型的界面，晶间ＳｉＣ颗粒与基体相的界面大部分是直接结合的。     

Single step fabrication of N-doped graphene/Si3N4/SiC heterostructures

In-plane heteroatom substitution of graphene is a promising strategy to modify its properties. The ability to dope graphene with electron-donor nitrogen heteroatoms is highly important for modulating electrical properties of graphene. Here we demonstrate a transfer-free method to directly grow large area quasi free-standing N-doped graphene bilayers on an insulating substrate （Si3N4）. Electron-bombardment heating under nitrogen flux results in simultaneous growth of N-doped graphene and a Si3N4 layer on the SiC surface. The decoupling of N-doped graphene from the substrate and the presence of Si3N4 are identified by X-ray photoemission spectroscopy and low-energy electron diffraction. The substitution of nitrogen atoms in the graphene planes was confirmed using high resolution X-ray photoemission spectroscopy which reveals several atomic configurations for the nitrogen atoms： Graphitic-like, pyridine-like, and pyrrolic- like. Furthermore, we demonstrated for the first time that N-doped graphene could be used to efficiently probe oxygen molecules via nitrogen atom defects.     

SiC和Si_3N_4粉体的太赫兹时域光谱研究

采用太赫兹时域光谱装置测试SiC和Si3N4粉体在0.4～2.4 THz的透射光谱,研究SiC和Si3N4粉体对太赫兹波的吸收性能与其电导率的关系,分析SiC和Si3N4粉体对太赫兹波的散射特性。结果表明,SiC是一种半导体材料,其内部含有较多可以自由移动的载流子,对太赫兹波的吸收较强;Si3N4是绝缘性很好的材料,对太赫兹波的吸收很小;SiC和Si3N4粉体对太赫兹波的散射作用属于瑞利散射,但是测试波长比粉体粒径大得多,散射效果不明显。     

Preparation and characterization of nano-structured monolithic SiC and Si3N4/SiC composite by hot isostatic pressing

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

Si3N4/SiC层状结构陶瓷摩擦磨损性能研究

利用Falex多重样品球-三块式的摩擦磨损试验机,重点研究了单层Si3N4陶瓷,9层和5层Si3N4/SiC层状结构陶瓷在不同的外加载荷、不同的界面应力分布大小、不同的表面组成与层状结构陶瓷的摩擦磨损性能的关系.结果表明:随着外加载荷逐渐加大,材料的耐磨损性能降低,表现为达到磨损突变点的时间缩短,磨痕直径变大;界面残余压应力对层状结构陶瓷耐磨损性能的提高起着重要的作用,9层结构陶瓷的界面残余压应力高出5层结构的层状陶瓷20%左右,表现出更高的耐磨损性能;SiC Si3N4两相复合陶瓷极大地提高了材料表面的耐磨损性能,在同样外加载荷下,表现为达到磨损突变点的时间更长,磨痕直径更小.     

Fabrication,mechanical properties and microstructure analysis of Si3N4/SiC nanocomposite

Ceramic nanocomposites, Si₃N₄ matrix reinforced with nano-sized SiC particles, were fabricated by hot pressing the mixture of Si₃N₄ and SiC fine powders with different sintering additives. Distinguishable increase in fracture strength at low and high temperatures was obtained by adding nano-sized SiC particles in Si₃N₄ with Al₂O₃ and/or Y₂O₃. Si₃N₄/SiC nanocomposite added with Al₂O₃ and Y₂O₃ demonstrated the maximum strength of 1.9 GPa with average strength of 1.7 GPa. Fracture strength of room temperature was retained up to 1400 as 1 GPa in the sample with addition of 30 nm SiC and 4 wt% Y₂O₃. Striking observation in this nanocomposite is that SiC particles at grain boundary are directly bonded to Si₃N₄ grain without glassy phases. Thus, significant improvement in high temperature strength in this nanocomposite can be attributed to inhibition of grain boundary sliding and cavity formation primarily by intergranular SiC particles, besides crystallization of grain boundary phase.     

Thermomechanically induced embrittlement in hot isostatically pressed Si3N4/SiC composites

The macroscopic fracture properties of an Si₃N₄/SiC-platelet composite fabricated by hot isostatic pressing (HIP) without sintering aids were measured by the chevron-notch technique in bending and related to micromechanisms of fracture by means of a quantitative profilometric analysis of the fracture surfaces. Compositional and processing parameters were varied systematically in order to maximize both the fracture toughness and the work of fracture of the composite. Data were compared with those of monolithic Si₃N₄ fabricated by the same process. Cooling-rate from the HI Ping temperature was indicated as a critical parameter especially when cooling was performed under high pressure. A marked embrittlement of the composite body was found by cooling at around 650 °C h^–1 and it could not be completely recovered by successive annealing even up to temperatures above 1700 °C. The highest fracture toughness and work of fracture in the composite (obtained at a cooling rate of about 100 °C h^–1), were measured as 4.6 MPa m^1/2 and 58.6 J m^–2, respectively. In agreement with fractal analysis results, they were estimated to be about 60%–70% of the maximum values, respectively, obtainable in the present composite system, provided that a complete debonding at the platelet/matrix interface can occur.     

Mechanical properties Of Si3N4 cerarnics reinforced with SiC whiskers and SiC platelets

Silicon nitride ceramics reinforced with SiC whiskers and SiC platelets were fabricated by hot pressing and their mechanical properties were studied. They showed higher fracture energy than conventional composites, particularly when they were consolidated by gas-pressure hot pressing at high temperature. A high fracture toughness (10.7 MPa m^1/2) which was measured by the single-edge pre-cracked beam method was achieved. Furthermore, a unique method to observe the crack propagation behaviours directly in a scanning electron microscope with loading devices was developed. As a result, much bridging and pull-out of the whiskers and the elongated Si₃N₄ grains, and crack deflection along the platelets, were observed behind the crack tip. This means that these grains are effective in enhancing the fracture resistance during crack propagation.     

Strength,toughness and R-curve behaviour of SiC whisker-reinforced composite Si3N4 with reference to monolithic Si3N4

The flexural strength and fracture toughness of 30 vol% SiC whisker-reinforced Si₃N₄ material were determined as a function of temperature from 25 to 1400°C in an air environment. It was found that both strength and toughness of the composite material were almost the same as those of the monolithic counterpart. The room-temperature strength was retained up to 1100°C; however, appreciable strength degradation started at 1200°C and reached a maximum at 1400°C due to stable crack growth. In contrast, the fracture toughness of the two materials was independent of temperature with an average value of 5.66 MPam^1/2. It was also observed that the composite material exhibited no rising R-curve behaviour at room temperature, as was the case for the monolithic material. These results indicate that SiC whisker addition to the Si₃N₄ matrix did not provide any favourable effects on strength, toughness and R-curve behaviour.     

Behaviour of SiC+Si3N4 mixtures during heating

This article discusses the behavior of the Si₃N₄+SiC mixture during sintering. The purpose of this study was to obtain data on sintered Si₃N₄/SiC composites. The proportion of Si₃N₄ and SiC powders in the initial mixtures varied from 0% to 100%, while the molar ratio of SiO₂/Y₂O₃ was 2:1 and the total amount of additives (14 wt.%) was kept constant. Samples of the powders were pressed under 300 MPa and heated to 1600, 1650, 1700, 1750, 1800, 1850, 1900, 1950 and 2000 °C, in a nitrogen atmosphere, and allowed to cool as soon as this temperatures were reached. After the heating step, the samples were characterized according to their final density, crystalline phases, microstructures and weight loss. The samples displayed little weight loss, but their density decreased with increasing amounts of SiC, particularly at temperatures above 1750 °C. All the mixtures showed the formation of liquid phase between 1650 and 1750 °C, regardless of their composition.