Green State Joining of SiC without Applied Pressure

External pressure (uniaxial or isostatic) is usually necessary to form a thin and defect-free joint in green state joining of SiC ceramics. A successful method of joining SiC in the green state using a liquid polymer precursor, allylhydridopolycarbosilane (AHPCS), without applied pressure, is described. The thermal decomposition behavior of the polymer was examined, and defect formation during joint evolution was investigated by interrupting the heat treatment at various stages. Cracks and pores were observed in the joints formed by pure AHPCS during the pyrolysis of the polymer precursor. Adding SiC powder to the joining paste eliminated defect formation. Optimum SiC loading in the paste was determined to be in the range of 25–35 vol%. Joints formed by AHPCS + (SiC + 5 wt% B) paste were essentially indistinguishable from the matrix and had an average strength of 323 MPa, comparable to that of the control sample.     

Evaluation of tribological behavior of silicon carbide and silicon nitride ceramics under different conditions

A comparative analysis of the tribological behavior of commercially available sintered silicon carbide (SiC) and three different types of silicon nitride (Si₃N₄) ceramics have been carried out using the ball-on-disk method in dry and lubrication (deionized [DI] water and ethanol) environment. Scanning electron microscopy (SEM) was used to understand the morphology and chemical composition of the tribo-surfaces. Sintered SiC (Hexoloy-SA) had the highest friction coefficient during dry sliding with an average of ∼0.34. Deionized water showed a minor improvement in friction (∼0.27) while ethanol reduced the friction greatly to ∼0.18 compared to dry sliding. During dry sliding, the presence of an abrasive third body was responsible for the high wear rates (WRs) in these compositions. Hexoloy-SA showed a lower WR during ethanol and DI water lubrication due to the formation of stable tribofilms as well as higher hardness which resisted the formation of third bodies. In comparison, Si₃N₄ samples showed a lower WR in DI water and ethanol. The samples also showed composition-dependent behavior which indicates that grain structure and grain boundary chemistry are playing a vital role in the tribological process.     

Rare earth (RE: Nd,Dy, Ho,Y, Yb,and Sc) aluminosilicates for joining silicon carbide components

Six different types of glass 12.18 RE₂O₃‐22 Al₂O₃‐65.82 SiO₂ (mol %) where RE: Nd, Dy, Ho, Y, Yb, and Sc were tested for joining silicon carbide (SiC) components. The different types of glass vary in their thermal properties but they are similar in their behavior for the joining process when a laser‐based heating technology was used. The quality of the joints was characterized by microscopic analysis, mechanical tests, and measurements of tightness. Annealing experiments were conducted at temperatures in the range of the glass transition and crystallization allowing an assessment of the compositions for usability as glass and as glass‐ceramic interlayers. Five of the investigated compositions can be recommended for application up to temperatures of 900°C. The Y‐ and Yb‐based compositions guarantee a high joint quality at temperatures up to 1200°C. The high temperature assessment was based on tightness and microstructural analyses of the joints after the annealing procedures. The results can be transferred to joining processes with lower heating and cooling rates.     

Diffusion bonding of SiC ceramics with interlayers of metallic titanium foils and PVD titanium coatings

Silicon carbide (SiC) is a candidate material for high-temperature structural aerospace applications due to its thermal and mechanical properties. Joining technologies enable the fabrication of complex shaped components needed for such applications. Various interlayers and processing conditions were used to form diffusion bonds between SiC substrates. Interlayers of titanium (Ti) foils and physically vapor deposited Ti coatings were used in the thicknesses of 10 and 20 μm with processing hold times of 1, 2, and 4 h. Polished cross sections of resulting diffusion bonds were analyzed using scanning electron microscopy (SEM) coupled with energy-dispersive spectroscopy (EDS) and using transmission electron microscopy (TEM). From the TEM analysis, selected-area diffraction patterns for Ti₃SiC₂, Ti₅Si₃C_x, and TiSi₂ were observed. Moreover, TiC and an unknown phase were present in diffusion bonds formed with metallic titanium foil. From the SEM/EDS analyses, intermediate phases of Ti₅Si₃C_x and TiC were found to be present in microcracked diffusion bonds. With the thinner Ti interlayers and/or longer processing time, microcracking was alleviated or eliminated due to the presence of the more stable and lower thermal expansive phases of Ti₃SiC₂ and TiSi₂. Detailed analysis of microstructures and the probable phases that formed in the bonded regions is presented.     

Electrical,thermal, and mechanical properties of porous silicon carbide ceramics with a boron carbide additive

The effects of the boron carbide (B₄C) content and sintering atmosphere on the electrical, thermal, and mechanical properties of porous silicon carbide (SiC) ceramics were investigated in the porosity range of 58.3%–70.3%. The electrical resistivities of the nitrogen-sintered porous SiC ceramics (∼10^–1 Ω·cm) were two orders of magnitude lower than those of argon-sintered porous SiC ceramics (∼10¹ Ω·cm). Both the thermal conductivities (3.3–19.8 W·m^–1·K^–1) and flexural strengths (8.1–32.9 MPa) of the argon- and nitrogen-sintered porous SiC ceramics increased as the B₄C content increased, owing to the decreased porosity and increased necking area between SiC grains. The electrical resistivity of the porous SiC ceramics was primarily controlled by the sintering atmosphere owing to the N-doping from the nitrogen atmosphere, and secondarily by the B₄C content, owing to the B-doping from the B₄C. In contrast, the thermal conductivity and flexural strength were dependent on both the porosity and necking area, as influenced by both the sintering atmosphere and B₄C content. These results suggest that it is possible to decouple the electrical resistivity from the thermal conductivity by judicious selection of the B₄C content and sintering atmosphere.     

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.     

Pressureless joining of SiC ceramics with magnesia-alumina-silica glass ceramics

Liquid phase sintered SiC ceramics were joined using magnesia-alumina-silica (MAS) glass-ceramic fillers without applied pressure. Four different filler compositions with 9.3–25.2 wt.% MgO, 20.7–33.6 wt.% Al₂O₃, and 49.2–68.1 wt.% SiO₂ were studied. The effects of filler composition and joining temperature (1450–1600°C) on the joint strength were investigated. All compositions exhibited an optimum joining temperature at which the maximum joint strength was obtained. A low joining temperature resulted in poor wetting of the SiC substrate due to the high viscosity of the filler. Whereas a high joining temperature caused dewetting and large unfilled sections in the interlayer due to the deleterious interfacial reactions. The joint strength was inversely proportional to the interlayer thickness, which was a function of filler composition and joining temperature. The SiC ceramic joined at 1525°C with MgO-25 wt.% Al₂O₃-60 wt.% SiO₂ filler exhibited a four-point bending strength of 286 ± 40 MPa.     

环氧树脂/碳化硅复合材料的热性能及韧性

采用碳化硅作为增强剂制备了环氧树脂/碳化硅复合材料,考察了复合材料的热学及力学性能。实验结果表明,碳化硅的添加使环氧树脂的玻璃化温度提高。当碳化硅添加质量分数为3%时,复合材料的韧性与纯环氧树脂相比提高了35%。     

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.     

Green State Joining of Silicon Carbide Using Polycarbosilane

Green state joining of SiC was investigated using a paste consisting of polycarbosilane polymer and SiC powder. The joining process and densification were described. Initial experiments resulted in the formation of symmetrical black bands and cracks on both sides of the joint. However, with modifications in processing conditions, the cracks were eliminated and the resulting joints were indistinguishable from the matrix. The flexural strength of joined samples was measured to be 234 MPa, which was comparable to that of the control sample with similar density. As the applied pressure during joining was increased from 34 to 138 MPa, the strength of the joined samples increased from 180 to 250 MPa.     

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.     

碳化硅晶片的制备技术

碳化硅晶须和晶片都是陶瓷基、金属基、树脂基复合材料的理想增强体，与碳化硅晶须相比，有关碳化硅晶片制备与应用的报道相对较少。论述了碳化硅晶片在复合材料中的应用，比较了国内外碳化硅晶片的各种制备技术。阐明了加热方式对碳化硅晶片制备的影响。指出低成本、新型热源的开发与推广应用有利于实现碳化硅晶片的规模化生产。     

Process-tolerant pressureless-sintered silicon carbide ceramics with alumina-yttria-calcia-strontia

Process-tolerant SiC ceramics were prepared by pressureless sintering at 1850–1950 °C for 2 h in an argon atmosphere with a new quaternary additive (Al₂O₃-Y₂O₃-CaO-SrO). The SiC ceramics can be sintered to a > 94% theoretical density at 1800–1950 °C by pressureless sintering. Toughened microstructures consisting of relatively large platelet grains and small equiaxed grains were obtained when SiC ceramics were sintered at 1850–1950 °C. The presently fabricated SiC ceramics showed little variability of the microstructure and mechanical properties with sintering within the temperature range of 1850–1950 °C, demonstrating process-tolerant behavior. The thermal conductivity of the SiC ceramics increased with increasing sintering temperature from 1800 °C to 1900 °C due to decreases of the lattice oxygen content of the SiC grains and residual porosity. The flexural strength, fracture toughness, and thermal conductivity of the SiC ceramics sintered at 1850–1950 °C were in the ranges of 444–457 MPa, 4.9–5.0 MPa m^1/2, and 76–82 Wm^?1 K^?1, respectively.     

Preparation of reaction bonded silicon carbide (RBSC) using boron carbide as an alternative source of carbon

RBSC composites are fully dense materials fabricated by infiltration of compacted mixtures of silicon carbide and carbon by molten silicon. Free carbon is usually added in the form of an organic resin that undergoes subsequent pyrolysis. The environmentally unfriendly pyrolysis process and the presence of residual silicon are serious drawbacks of this process. The study describes an alternative approach that minimizes the residual silicon fraction by making use of a multimodal particle size distribution, in order to increase the green density of the preforms prior infiltration. The addition of boron carbide provides an alternative source of carbon, thereby eliminating the need for pyrolized organic compounds. The residual silicon fraction in the RBSC composites, prepared according to the novel processing route, is significantly reduced. Their mechanical properties, in particular the specific flexural strength is by 15% higher than the value reported for RBSC composites prepared by the conventional approach.     

竹节状碳化硅晶须吸波性能研究

采用电磁波吸收材料来降低电磁波对设备的干扰及对人体的伤害,是目前常用的电磁波防护手段之一。特定结构碳化硅晶须作为一种一维介电材料,其优于普通的晶须、块状和颗粒状的吸波性能引起了研究人员的关注。本研究以生竹粉、硅粉和二氧化硅为原料,通过碳热还原法在不同温度下制备了竹节状碳化硅晶须,并对其结构和吸波性能进行了检测分析。结果表明：以1400℃烧结的竹节状晶须制备的试样在厚度为3 mm,频率为9.1 GHz时,最小反射损耗达到-14.4 dB,有效吸收带宽为1.8 GHz,吸波性能最好,具有进一步研究价值。     

反应烧结碳化硅高温性能的研究进展

反应烧结碳化硅具有优良的力学性能、抗侵蚀性能和抗氧化性能等优点,是一种高致密度、低成本和净尺寸成型的材料.但由于反应烧结法的特殊工艺,反应烧结碳化硅中常含有较多游离硅,严重损害了材料的高温性能.主要阐述了反应烧结碳化硅高温力学性能、抗氧化性能、导热性能和抗热震性能的研究现状,并总结了近年来降低游离硅含量、提高反应烧结碳...     

碳化硅陶瓷固相烧结的烧结机理及研究进展简

碳化硅陶瓷材料具有高硬度、高强度、抗氧化、耐高温、高热导率、低线胀系数等优良性能,同时具有优良的化学稳定性且能够耐大多数种类的酸碱溶液腐蚀,在石油、化工、建材、航空、机械等诸多领域得到了广泛应用。本文主要阐述了碳化硅陶瓷固相烧结的烧结机理,并对目前国内外关于碳化硅陶瓷固相烧结的研究进展进行了阐述。     

Thermal shock resistance and hoop strength of triplex silicon carbide composite tubes

Multi‐layered SiC composites have been considered as a nuclear fuel cladding material of light water reactors, LWRs, because of their excellent high temperature strength and corrosion resistance under accident conditions. During a design basis accident of a LWR such as a loss‐of‐coolant accident, the peak temperature of the fuel clad rapidly increases as the production of decay heat continues. The emergency core cooling systems then automatically supply the reactor core with emergency cooling water. The fuel clad consequently suffers from thermal shock. In this study, the structural integrity of multi‐layered SiC composite tubes after thermal shock was investigated. Several kinds of multi‐layered SiC composite tubes consisting of CVD SiC and CVI SiC_f/SiC were water‐quenched from 1200°C to room temperature. The triplex SiC composite tube retained its tubular geometry during quenching. The strength degradation after thermal shock was <13% for the specimens with a PyC interphase. The residual stress distribution within the tubes during thermal shock was evaluated by a finite element method.     

Low-temperature sintering of single-phase,high-entropy carbide ceramics

Dense (Hf, Zr, Ti, Ta, Nb)C high-entropy ceramics were produced by hot pressing (HP) of carbide powders synthesized by carbothermal reduction (CTR). The relative density increased from 95% to 99.3% as the HP temperature increased from 1750°C to 1900°C. Nominally phase pure ceramics with the rock salt structure had grain sizes ranging from 0.6 µm to 1.2 µm. The mixed carbide powders were synthesized by high-energy ball milling (HEBM) followed by CTR at 1600°C, which resulted in an average particle size of ~100 nm and an oxygen content of 0.8 wt%. Low sintering temperature, high relative densities, and fine grain sizes were achieved through the use of synthesized powders. These are the first reported results for low-temperature densification and fine microstructure of high-entropy carbide ceramics.     

High thermal conductivity of spark plasma sintered silicon carbide ceramics with yttria and scandia

A fully dense SiC ceramic with a room‐temperature thermal conductivity of 262 W·(m·K)^?1 was obtained via spark plasma sintering β‐SiC powder containing 0.79 vol% Y₂O₃‐Sc₂O₃. High‐resolution transmission electron microscopy revealed two different SiC‐SiC boundaries, that is, amorphous and clean boundaries, in addition to a fully crystallized junction phase. A high thermal conductivity was attributed to a low lattice oxygen content and the presence of clean SiC‐SiC boundaries.