Bonding of Dense Silicon Nitride with Carbon Interlayers

Diffusion bonding of dense Si₃N4 containing 10% Ce₂O₃, 7% A1₂O₃, and 2% Y₂O₃ was attempted through hot pressing at temperatures of 1000° to 1400°C. Physically vapor-deposited (PVD) carbon and paraffin-wax candle soot were tried as interlayers. The interfaces were analyzed through optical and scanning electron microscopy, and through X-ray photoelectron spectroscopy. The bonding temperature could be reduced from 1400° (without interlayers) to 1100°C with PVD carbon or candle soot. From C Is and Si 2p spectra, the formation of SiC at the interface through the reaction of C with the silicon oxynitride layer has been identified.     

Silicon Nitride Joining Using Silica and Yttria Ceramic Interlayers

Dense hot-pressed β-Si₃N₄ blocks were joined using both SiO₂ and SiO₂-Y₂O₃ powder slurries as bonding interlayers. The assembled specimens (Si₃N₄/interlayer/Si₃N₄) were heated in a flowing N₂ atmosphere in the temperature range of 1500°–1650°C. The joining interlayer was clearly distinguished from the Si₃N₄ bulk. The microstructure and the reaction products found in the bonding interlayer were very different in both compositions. Reactions occurring between the Si₃N₄ and the ceramic joining compositions have been explained based on existing diagrams of the YN–Si₃N₄-Y₂O₃-SiO₂ system.     

Seamless Joining of Silicon Nitride Ceramics

High-strength joining of Si₃N₄ ceramics has been achieved by developing a process that effectively eliminates the seam, and may allow for fabrication of large or complex silicon nitride bodies. This approach to joining is based on the concept that when sintering aids are effective in bonding individual grains, they could be equally effective in joining bulk pieces of Si₃N₄. Optimization of the process led to Si₃N₄/Si₃N₄ joints with room-temperature bend strengths as high as 950 MPa, corresponding to more than 90% of the bulk strength of the Si₃N₄. At elevated temperatures of 1000° and 1200°C joint strengths of 666 and 330 MPa, respectively, were obtained, which are the highest values reported to date for these temperatures. These bend strengths are also more that 90% of the strength of bulk Si₃N₄ measured at these temperatures.     

Liquid-Phase Bonding of Silicon Nitride Ceramics

Mg-Si-O-N glasses were used to bond dense Si₃N₄ ceramic pieces by a liquid-phase diffusion bonding mechanism. In this case, it was difficult to achieve defect-free bonding because, at low nitrogen content in the glass, a large mismatch in thermal expansion coefficient produced cracks perpendicular to the bonding glass layer. With an increase in nitrogen content, the glass layer became frothy and contained "bubbles." However, when a small amount of elemental silicon was added to the glass, volatile reaction was suppressed and intimate bonding was achieved without thermal cracks.     

Bonding Mechanisms in Silicon Nitride Brazing

We investigated the wetting behavior and reactions of different metals on Si₃N₄ using sessile drop measurements, analysis of reaction layers, and measurements of strengths of joined bars. Active metals, such as Al and Ti, and alloys that contain them react with Si₃N₄ and cause wetting and spreading at the interface. Al-Si₃N₄ reaction at 900°C produced a thin layer of Al₂O₃ at the interface. Reaction between Si₃N₄ and Ag-Cu-To braze alloys at 900°C resulted in a complex microstructure in the reaction zone that contained TiN and titanium silicides. Breaking strengths of Si₃N₄ bars joined with the Ag-Cu-Ti braze alloys were higher than those for Si₃N₄ joined with Al, primarily because of the better wetting by the Ag-Cu-Ti alloys. Nonreactive metals and alloys such as Sn, In, Ag-Cu, and Ag-Cu-Sn neither wet, spread, nor adhere to Si₃N₄ substrates.     

Si3N4陶瓷烧结中烧结助剂的研究进展

研究了多种烧结助剂对氮化硅烧结性能和烧结过程的影响.研究表明,多组分助剂比单一组分助剂对氮化硅的助烧效果好,其中稀土氧化物和MgO-Al2O3-SiO2体系比较受重视.     

氧化锆复合氮化硅陶瓷

分析了二氧化锆的性质及氧空位对二氧化锆相变的影响 ,讨论了二氧化锆韧化氮化硅陶瓷的影响因素 ,提出了二氧化锆韧化氮化硅陶瓷时避免氮化锆生成、促进复相氮化硅陶瓷烧结的途径。     

氮化硅常压烧结研究进展

本文着重论述了氮化硅陶瓷常压烧结过程中助烧剂的选择、烧结机理和高温性能的改善方面的研究进展。     

低温放电等离子烧结法制备氮化硅陶瓷

分别以MgO-Al2O3或MgO-AlPO4作为烧结助剂,采用放电等离子体低温快速烧结方法制备了主相为α相的Si3N4陶瓷材料.采用X射线衍射和扫描电子显微镜分析了样品的物相组成和显微结构;研究了烧结助剂及其含量、烧结温度对陶瓷样品的相对密度与力学性能的影响.结果表明:当采用4%质量分数,下同)MgO-4%Al2O3烧...     

Push-Pull Fatigue of Sintered Silicon Nitride Ceramics at Elevated Temperatures

The fatigue tests under push-pull completely reversed loading and pulsating loading were performed for silicon nitride ceramics at elevated temperatures. Then the effects of stress wave form, stress rate, and cyclic understressing on fatigue strength, and cyclic straining behavior, were examined. The cycle-number-based fatigue life is found to be shorter under trapezoidal stress wave loading than under triangular stress wave loading, and to become shorter with increasing hold time under the trapezoidal stress wave loading. Meanwhile, the equivalent time-based life curve, which is estimated from the concept of slow crack growth, almost agrees with the static fatigue life curve in the short and intermediate life regions, showing the small cyclic stress effect and the dominant stress-imposing period effect on cyclic fatigue life. The fatigue strength increased in stepwise stress amplitude increasing test, where stress amplitude is increased stepwise every given number of stress cycles, at 1100° and 1200°C. Occurrence of cyclic strengthening was proved through a gradual decrease in strain amplitude during a pulsating loading test at 1200°C in this material, corresponding to the above cyclic understressing effect on fatigue strength.     

Oxidation and Fracture Strength of High-Purity Reaction-Bonded Silicon Nitride

Reaction-bonded Si₃N₄ (RBSN) made from high-purity Si powder is unusually resistant to degradation caused by exposures to air for up to 50 h at temperatures up to 1400°C. The weight gain during oxidation of this SiH₄-originating RBSN is approximately 10 times less than conventional RBSN. Contrary to normally observed strength degradations, room-temperature strengths of this high-purity, oxidized RBSN (avg = 435 MPa, max. = 668 MPa) remained at their unusually high, as-processed levels after 1000° and 1400°C oxidizing exposures. Fracture toughness values were unaffected by oxidation ( K _IC= 2.3 to 2.4 MPa · m^1/2). This superior oxidation resistance results from the high purity and the small diameter pore channels (0.01 to 0.06 μm) achieved in this SiH₄-originating RBSN.     

Effect of Bonding Pressure on Silicon Nitride Joining Using a Nickel-Chromium-Boron Metal Filler

Mechanical pressure exerts a noticeable effect on the reaction that takes place at the interfacial region of Si₃N₄/Ni-Cr-B/Si₃N₄ joints. In fact, the mechanical pressure affects the thickness of the reaction layer: for lower pressures, a large interfacial reaction layer and a profusion of cracks are observed, whereas, for higher pressures, the extent of the reaction layer is limited, and no cracks are detected. The results show that joint strength increases monotonically with applied pressure.     

Layered Silicon Nitride-Based Composites with Discontinuous Boron Nitride Interlayers

The influence of a strong/weak interface ratio on the mechanical properties of Si₃N₄/BN-based layered composites was studied. The ratio was controlled by the number of BN spots between the adjacent Si₃N₄ layers. By increasing the BN interface area from 0% to 72%, fracture toughness increased from 7.7 to 10.9 MPa·m^1/2, and bending strength decreased from 1275 to 982 MPa. Fracture toughness was improved from 8.6 to 10.1 MPa·m^1/2 by additional heat treatment of samples containing 2 vol%β-Si₃N₄ seed particles. The bending strength of samples with 35% weak BN interfaces, measured perpendicular and parallel to layer alignment, was 1260 and 1240 MPa, respectively. This confirmed the two-directional isotropy of layered samples.     

烧结助剂对氮化硅陶瓷显微结构和性能的影响

氮化硅中氮原子和硅原子的自扩散系数很低，致密化所必需的扩散速度和烧结驱动力都很小，在烧结过程中需采用烧结助剂。烧结助剂是影响氮化硅陶瓷的显微结构和性能的关键因素之一。有效的烧结助剂不但可以改善氮化硅陶瓷的显微结构，而且可以提高氮化硅陶瓷的高温性能和抗氧化性能。     

无压烧结氮化硅陶瓷的物理性能研究

以α-Si₃N₄粉末为原料,Y₂O₃和MgAl₂O₄体系为烧结助剂,采用无压烧结方式,研究了烧结温度、保温时间、烧结助剂含量以及各组分配比对氮化硅致密化及力学性能的影响。结果表明:以Y₂O₃和MgAl₂O₄为烧结助剂体系,氮化硅陶瓷在烧结温度为1 600 ℃,保温时间为4 h,烧结助剂含量为12.5%(质量分数),Y₂O₃和MgAl₂O₄质量比为1∶1时,综合性能最好;氮化硅陶瓷显气孔率为0.21%,相对密度为98.10%,抗弯强度为598 MPa,维氏硬度为15.55 GPa。     

Computer Simulation of the Microstructure Developed in Reaction-Sintered Silicon Nitride Ceramics

A simulation model of the microstructure developed during the reaction sintering of ultrafine silicon powders is presented. The model employs interactive subroutines that describe particle compaction, sintering, and nitridation. The particle compaction model is based on a random particle packing model, whereas the sintering and reaction sintering models are based on the modified grain model and the sharp interface model (SIM). Microstructural changes due to the competition between chemical reaction and sintering are taken into account in the model. The results predicated by this model show good agreement with experimental data from previous studies.     

Silicon Nitride Oxidation Based on Oxynitride Interlayers with Graded Stoichiometry

The oxidation kinetics of Si₃N₄ were modeled by describing the simultaneous diffusion and reaction of interstitial oxygen that is believed to occur inside of the silicon oxynitride interlayer. The oxynitride was assumed to have a variable composition, and oxidation was described as a reaction where interstitial oxygen is incorporated into the network structure of the oxynitride and nitrogen is removed. It was assumed that both the diffusion coefficient and the solubility of interstitial oxygen decrease as the nitrogen content of the network structure increases. The results accurately describe both the formation of an oxynitride layer during oxidation, and the relatively slow oxidation kinetics of Si₃N₄ (compared to Si and SiC).     

低温无压烧结氮化硅陶瓷的相变及致密化研究

采用氧化铝（Al2 O3）和氧化钇（Y2 O3）为烧结助剂,利用无压烧结工艺在低温下制备氮化硅陶瓷材料。利用XRD和SEM等着重研究了无压烧结氮化硅陶瓷低温阶段时的物相组成及其致密化。结果表明：当添加剂含量为10％,烧结温度高于1430℃时,α→β相转变较快;当烧结温度达到1510℃时,α相全部转变为β相。     

Interfacial Bonding and Friction in Silicon Carbide [Filament]-Reinforced Ceramic- and Glass-Matrix Composites

Interfacial shear strength and interfacial sliding friction stress were assessed in unidirectional SiC-filament-reinforced reaction-bonded silicon nitride (RBSN) and borosilicate glass composites and 0/90 cross-ply reinforced borosilicate glass composite using a fiber pushout test technique. The interface debonding load and the maximum sliding friction load were measured for varying lengths of the embedded fibers by continuously monitoring the load during debonding and pushout of single fibers in finite-thickness specimens. The dependences of the debonding load and the maximum sliding friction load on the initial embedded lengths of the fibers were in agreement with nonlinear shear-lag models. An iterative regression procedure was used to evaluate the interfacial properties, shear debond strength (T _d ), and sliding friction stress (T _f ), from the embedded fiber length dependences of the debonding load and the maximum frictional sliding load, respectively. The shear-lag model and the analysis of sliding friction permit explicity evaluation of a coefficient of sliding friction (μ) and a residual compressive stress on the interface (σ₀). The cross-ply composite showed a significantly higher coefficient of interfacial friction as compared to the unidirectional composites.     

Si3N4／Si3N4陶瓷连接的研究进展

本文综述了Ｓｉ３Ｎ４／Ｓｉ３Ｎ４陶瓷连接的研究现状，论述不同连接工艺对接头强度的影响。