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.     

Joining of Self-Bonded Silicon Carbide by Germanium Metal

Two self-bonded SiC bodies containing free Si were joined with liquid Ge at 1180°C in vacuum. Bond strength was measured by four-point bending test in vacuum at high temperature. The join had a significant strength even above the melting point of Ge metal. Electron probe microanalysis of joint showed a liquid formation temperature of thinner interlayer was ∼1200°C.     

In Situ Formation of Silicon Carbide Nanofibers on Cordierite Substrates

Twenty-five years of diesel particulate filter (DPF) developments have shown that high-volume ceramic materials are well suited for the harsh requirements of exhaust after treatment. Nevertheless, problems regarding filter reliability and durability associated with the regeneration of the filter have limited their serious application until only recently. To extend useful filter life, the present study has examined the growth of silicon carbide (SiC) nanofibers by a simple carbothermal reduction process on cordierite support surfaces using cheap raw materials such as kaolin, talc, and carbon black. Transmission electron microscopy confirms the crystalline (β - SiC) nature of the nanofibers (10–20 nm diameter). The growth of these nanofibers increases the support-specific surface area restricting the agglomeration of noble metal catalyst particles that otherwise occurs in wash-coat sintering. As a result, fewer particles are needed to perform the catalyst role (at reduced cost) and the support structure can host the catalyst for prolonged times at higher temperatures. As the future will see increasing economic competition in filter fabrication routes and materials, this new design of catalytic DPF promises to play a significant role.     

Thermodynamic Brazing Alloy Design for Joining Silicon Carbide

Using solution thermodynamic theory, a Ni-Cr Si alloy, based on the Ni/Cr ratio of AWS BNi-5 (Ni-18Cr-19Si (atom%)), was designed for brazing SiC ceramics. The optimum thermodynamic composition was computed to be Ni-14.3Cr-36Si (atom%). Brazing experiments were conducted to assess the effect of changing the Si content away from this composition on the joint microstructures. For alloys containing less than 36 atom% Si, an excessively vigorous joining reaction occurred, resulting in the formation of a porous reaction zone at the brazing alloy/SiC interface, the amount of porosity decreasing as the brazing alloy composition approached the thermodynamically predicted optimum. It was found that the most likely mechanism for the formation of the porous zone was CO evolution during the SiC decomposition reaction. The best microstructures were attained for 40 atom% Si alloy joints, closely agreeing with the thermodynamic model, whereas higher Si content alloys exhibited localized debonding of the brazing alloy from the SiC.     

碳化硅/堇青石复相多孔陶瓷的制备及性能研究

采用碳化硅、烧高岭土、氢氧化铝、滑石为主要原料,石墨为造孔剂制备了碳化硅/堇青石复相多孔陶瓷.研究了烧结温度和烧结助剂二氧化铈对碳化硅/堇青石复相多孔陶瓷气孔率和强度的影响,并分别用XRD和SEM分析晶相组成和断面显微结构表明:制备出的SiC多孔陶瓷的主相是SiC,结合相是堇青石与方石英,多孔陶瓷具有相互连通的开孔结构;在1350℃烧结,并保温3h,当造孔剂含量为15％时,碳化硅/堇青石复合多孔陶瓷性能最佳,其气孔率31.80％,相应的弯曲强度为63.74 MPa.在1200℃下,添加不同含量的CeO2,对烧结样品的相组成有影响,能够降低生成堇青石的温度,在CeO2含量为3％的样品中,堇青石的峰最明显,但是过量的氧化铈会抑制了堇青石的生成;随着CeO2加入量的增加,其气孔率和弯曲强度也会随之变化,1200℃下,在CeO2加入量为4％时其弯曲强度最优.但随着CeO2的含量的增加,其气孔率逐渐下降.     

Joining of Silicon Carbide/Silicon Carbide Composites and Dense Silicon Carbide Using Combustion Reactions in the Titanium–Carbon–Nickel System

A new ceramic joining technique has been developed that utilizes an exothermic combustion reaction to simultaneously synthesize the joint interlayer material and to bond together the ceramic workpieces. The method has been used to join SiC/SiC composites and dense SiC ceramics using TiC-Ni powder mixtures that ignite below 1200°C to form a TiC-Ni joining material. Thin layers of the powder reactants were prepared by tape casting, and joining was accomplished by heating in a hot-press to ignite the combustion reaction. During this process, localized exothermic heating of the joint region resulted in chemical interaction at the interface between the TiC-Ni and the SiC ceramic that contributed to bonding. Room-temperature four-point bending strengths of joints produced by this method have exceeded 100 MPa.     

Modified Tape Casting Method for Ceramic Joining: Application to Joining of Silicon Carbide

A simple modified tape casting procedure has been developed for application to ceramic joining when the joining materials are in powder form. The method involves preparation of a slurry from the powder, solvent, and thermoplastic binder, and then casting directly onto the joining surface using a moving doctor blade. Handling of the tape prior to joining is not necessary: therefore, binder content is minimized, plasticizers are not required, and viscosity is controlled by solvent content. The utility of this technique for producing joints with thin, uniform interlayers is demonstrated for silicon carbide materials joined with TiC + Ni and SiC + Si.     

Thermal Conductivity of Vapor-Liquid-Solid and Vapor-Solid Silicon Carbide Whisker-Reinforced Lithium Aluminosilicate Glass-Ceramic Composites

The thermal conductivities of two lithium aluminosilicate glass-ceramic matrix composites reinforced with 30 vol% of either SiC VS (rice hull) whiskers or SiC VLS (vapor-liquid-solid) whiskers were determined from room temperature to 500°C. Because of the preferred alignment of the whiskers, the thermal conductivity values normal to the hot-pressing direction were found to be significantly higher than those in the parallel direction. The composites with the VLS whiskers exhibited higher thermal conductivity values than those with the VS whiskers. An analysis of the room-temperature data showed that the thermal conductivity values parallel to the hot-pressing direction were higher than those predicted from theory, even for whiskers with infinite thermal conductivity and perfect interfacial thermal contact. This effect was attributed to a significant contribution of percolation to the total heat flow as a result of direct whisker-to-whisker contact. For both types of whiskers, the interfacial thermal conductance and thermal conductivity values (at ∼6.5 × 10⁵ W/(m²-K) and 200 W/(m·K), respectively) inferred from the composite thermal conductivity values perpendicular to the hot-pressing direction were essentially the same. It was concluded that the order of magnitude difference in thickness for the two whisker types was primarily responsible for the differences in thermal conductivity measured for these two composites.     

堇青石/碳化硅复相陶瓷窑具抗氧化性能研究

本文对碳化硅、堇青石的优点整合制备碳化硅/堇青石复相陶瓷窑具,以力学性能变化为基础通过研究偏钒酸铵含量、金属硅粉含量、烧成温度等3个方面对堇青石/碳化硅复相窑具材料抗氧化性能进行研究分析,并通过X-射线衍射(XRD)分析,复相陶瓷窑具中并未有明显的氧化物如SiO2等杂质相出现。     

Comparative Single-Point Diamond Scratching Behavior of a Cordierite Glass and Glass-Ceramic

A comparative study was conducted of the single-point diamond scratching response of a cordierite glass and glass-ceramic. For the glass, deformation and material removal occurred by viscous flow at the lowest values of load, viscous flow combined with crack formation adjacent to the contact area over the intermediate load range, and extensive spoiling at the highest values of load. The density of the spalls and spall size were found to be proportional and inversely proportional to perpendicular scratching load, respectively. The glass-ceramic exhibited plastic flow and abrasive wear at loads as low as could be reliably measured, the particle size of the debris being of the order of the grain size. At the highest ranges of load, the glass-ceramic exhibited material removal by spall formation with a spall size proportional to load. At the lower ranges of load, the widths of the scratch for the glass and glass-ceramic were comparable. However, at the highest values of load tne size of the spall of the glass-ceramic was significantly less than the size of the spall in the glass.     

Nano-Scale Cordierite Glass-Ceramic from Natural Raw Materials with Different Fluoride Additions

Silicon - Stable cordierite glass-ceramics were prepared from natural kaolin, silica sand and magnesite as raw materials. Furthermore the effect of fluorine additions was tested by addingAlF3 or...     

X-ray Tomography Study on Green State Joining of Silicon Carbide Using Polymer Precursors

X-ray tomography has been used to investigate the density variations in SiC joints formed using polymer pastes. It has been demonstrated that X-ray tomography provides accurate bulk density measurements and volumetric density gradients. The results suggest that the magnitude of the applied pressure after green state joining and the amount of polymer (polycarbosilane, PCS) in the joining pastes influence the green density of the joints. All joints are prepared and applied in air atmosphere and at room temperature. The green densities of the joints increase from 54% to 66% of theoretical with the increase of the applied pressure from ambient to 138 MPa. Highest joint density without applied pressure is achieved using paste containing 50 vol% PCS. Furthermore, allylhydridopopolycarbosilane- (AHPCS-) containing pastes resulted in higher densities at the joint–matrix interface, indicating infiltration of polymer into the matrix.     

Silicon Carbide Platelet/Silicon Carbide Composites

α-silicon carbide platelet/β-silicon carbide composites have been produced in which the individual platelets were coated with an aluminum oxide layer. Hot-pressed composites showed a fracture toughness as high as 7.2 MPa·m^1/2. The experiments indicated that the significant increase in fracture toughness is mainly the result of crack deflection and accompanying platelet pullout. The coating on the platelets also served to prevent the platelets from acting as nucleation sites for the α- to β-phase transformation, so that the advantageous microstructure remains preserved during high-temperature processing.     

Silicon Carbide/Silicon and Silicon Carbide/Silicon Carbide Composites Produced by Chemical Vapor Infiltration

Composites of SiC/Si and SiC/SiC were prepared from single yarns of SiC. The use of carbon coatings on SiC yarn prevented the degradation normally observed when chemically vapor deposited Si is applied to SiC yarn. The strength, however, was not retained when the composite was heated at elevated temperatures in air. In contrast, the strength of a SiC/C/SiC composite was not reduced after this composite was heated at elevated temperatures, even when the fiber ends were exposed.     

Silicon Carbide Monofilament-Reinforced Silicon Nitride or Silicon Carbide Matrix Composites

SiC-monofilament-reinforced SiC or Si₃N₄ matrix composites were fabricated by hot-pressing, and their mechanical properties and effects of filaments and filament coating layers were studied. Relationships between frictional stress of filament/matrix interface and fracture toughness of SiC monofilament/Si₃N₄ matrix composites were also investigated. As a result, it was confirmed experimentally that in the case of composites fractured with filament pullout, the fracture toughness increased as the frictional stress increased. On the other hand, when frictional stress was too large (>about 80 MPa) for the filament to be pulled out, fracture toughnesses of the composites were almost the same and not so much improved over that of Si₃N₄ monolithic ceramics. The filament coating layers were found to have a significant effect on the frictional stress of the SiC monofilament/Si₃N₄ matrix interface and consequently the fracture toughness of the composites. Also the crack propagation behavior in the SiC monofilament/Si₃N₄ matrix composites was observed during flexural loading and cyclic loading tests by an in situ observation apparatus consisting of an SEM and a bending machine. The filament effect which obstructed crack propagation was clearly observed. Fatigue crack growth was not detected after 300 cyclic load applications.     

Microstructure and Fracture Toughness of Hot-Pressed Silicon Carbide Reinforced with Silicon Carbide Whisker

The effects of β-SiC whisker addition on the microstructural evolution and fracture toughness ( K _IC) of hot-pressed SiC were investigated. Most of the whiskers added disappeared during the densifcation process by transformation into the α-phase. The remaining whiskers acted as nuclei for grain growth, resulting in the formation of large tabular grains around the whiskers. The tabular grains around the whiskers were believed to be formed because of the extreme anisotropy of the interfacial energy between α- and β-SiC. The K _IC of the material was improved significantly by the whisker addition. The increase in the K _IC was attributed to crack bridging followed by grain pullout as a result of the formation of tabular grains in a fine matrix.     

Microstructure and Mechanical Properties of SiC Platelet/Cordierite Glass-Ceramic Composites

Cordierite glass-ceramics reinforced with different volume fractions (0, 10, 20, and 30%) of SiC platelets were fabricated by mechanically mixing appropriate powders and hot pressing above the glass transition temperature. Some of the specimens were subjected to postsintering crystallization treatments. The resultant sintered microstructure was textured, and within it the SiC platelets tended to be oriented with their basal planes perpendicular to the hot-pressing direction. The bending strength of the hot-pressed specimens was constant, while the fracture toughness increased with the SiC content. Crystallization heat treatment in argon for 30 min at 1200°C caused a significant decrease in the bending strength, but improved the fracture toughness. Fractography has confirmed the crack deflection to be a dominant mechanism in the crystallized specimens, which contributes to the improvement in the fracture toughness. The overall changes in the mechanical properties are discussed with respect to the change in the residual stresses and oxidation characteristics of the SiC platelets.     

Silicon Nitride Joining

Hot-pressed Si₃N₄ was joined using an Mgo-A1₂O₃-SiO₂ glass composition chosen to approximate the oxide portion of the grain-boundary phase in the ceramic. After it has been heated at 1550° to 1650°, the interface of the joined ceramic is an interlocking mixture of Si₂N₂O, β-Si₃N₄, and a residual oxy-nitride glass. The kinetics of reactions between Si₃N₄ and the molten joining composition were studied by X-ray diffraction analysis of the phases present in Si₃N4 powder-glass mixtures quenched after varied heat treatments. Analytical transmission electron microscopy of the composition and micro-structure of the reaction zone in joined specimens, together with the X-ray diffraction results, suggests that the driving force for joining is the lowering of the Si₃N₄ interfacial energy when it is wet by the molten silicate, augmented by the negative Gibbs energy for the reaction SiO₂( l ) + Si₃N₄= 2Si₂N₂O.     

Effects of Joining Pressure and Deformation on the Strength and Microstructure of Diffusion-Bonded Silicon Carbide

The effects of joining pressure and deformation on the strength and microstructure of diffusion-bonded SiC were examined using a hot-press to apply varying amounts of interfacial pressure and a close-fitting die to restrict deformation. SiC substrates were successfully diffusion bonded at 1950° and 2100°C. Joints which had uniform grain structure across the joint interface and bend strengths up to 300 MPa (44 ksi) were achieved. Pressing pressure was found to be a requirement for producing reasonable joint strength. It was also found that macroscopic deformation (>4% joint area expansion) is not necessary for effective diffusion bonding. Various methods for joining SiC are reviewed with regard to ease of processing, use limitations, and joint strength.     

Stress-Corrosion Cracking of Silicon Carbide Fiber/Silicon Carbide Composites

Ceramic-matrix composites are being developed to operate at elevated temperatures and in oxidizing environments. Considerable improvements have been made in the creep resistance of SiC fibers and, hence, in the high-temperature properties of SiC fiber/SiC (SiC_f/SiC) composites; however, more must be known about the stability of these materials in oxidizing environments before they are widely accepted. Experimental weight change and crack growth data support the conclusion that the oxygen-enhanced crack growth of SiC_f/SiC occurs by more than one mechanism, depending on the experimental conditions. These data suggest an oxidation embrittlement mechanism (OEM) at temperatures <1373 K and high oxygen pressures and an interphase removal mechanism (IRM) at temperatures of ≳700 K and low oxygen pressures. The OEM results from the reaction of oxygen with SiC to form a glass layer on the fiber or within the fiber–matrix interphase region. The fracture stress of the fiber is decreased if this layer is thicker than a critical value ( d > d _c) and the temperature below a critical value ( T < T _g), such that a sharp crack can be sustained in the layer. The IRM results from the oxidation of the interfacial layer and the resulting decrease of stress that is carried by the bridging fibers. Interphase removal contributes to subcritical crack growth by decreasing the fiber-bridging stresses and, hence, increasing the crack-tip stress. The IRM occurs over a wide range of temperatures for d < d _c and may occur at T > T _g for d > d _c. This paper summarizes the evidence for the existence of these two mechanisms and attempts to define the conditions for their operation.