In Situ-Toughened Silicon Carbide

A new processing strategy based on atmospheric pressure sintering is presented for obtaining dense SiC-based materials with microstructures consisting of (i) uniformly distributed elongate-shaped α-SiC grains and (ii) relatively high amounts (20 vol%) of second-phase yttrium aluminum garnet (YAG). This strategy entails the sintering of β-SiC powder doped with α-SiC, Al₂O₃, and Y₂O₃. The Al₂O₃ and Y₂O₃ aid in the liquid-phase sintering of SiC and form in situ YAG, which has a significant thermal expansion mismatch with SiC. During a subsequent grain-growth heat treatment, it is postulated that the α-SiC "seeds" assist in controlling in situ growth of the elongated α-SiC grains. The fracture pattern in the in situ -toughened SiC is intergranular with evidence of copious crack-wake bridging, akin to toughened Si₃N₄ ceramics. The elongate nature of the α-SiC grains, together with the high thermal-residual stresses in the microstructure, enhance the observed crack-wake bridging. This bridging accounts for a measured twofold increase in the indentation toughness of this new class of in situ -toughened SiC relative to a commercial SiC.     

Flexural Creep of an in Situ-Toughened Silicon Carbide

Flexural creep behavior is reported for an in situ -toughened SiC between 1100° and 1500°C in four-point bending. The flexural creep rate of this SiC, sintered with aluminum, boron, and carbon (ABC-SiC), exhibits linear stress dependence, low apparent activation energy, and low incidence of cavitation and dislocation production. Most grain boundaries in this ceramic contain 1–5 nm intergranular films. The creep rate is consistent with a grain-boundary transport mechanism involving diffusion along the grain-boundary film-SiC interfaces. The microstructure and grain boundaries have been examined using transmission electron microscopy to assess possible changes during creep, particularly in relation to the applied stress direction.     

Crack-Growth Resistance of in Situ-Toughened Silicon Nitride

The fracture toughness of a commercial, hot-pressed, in situ -toughened silicon nitride with an elongated grain structure is determined by four different testing methods. The fracture toughness is found to be 5.76 ± 0.27, 8.48 ± 0.50, 10.16 ± 0.66, and 10.68 ± 0.39 Mpa.m^1/2, respectively, by indentation crack size measurement, indentation strength, single-edge-precracked-beam, and chevron-notched-beam methods. The discrepancy in fracture toughness between the testing methods is related to R -curve behavior, as measured using the indentation strength technique. These results indicate that there is no unique fracture toughness value and that a fracture toughness testing method with appropriate qualifiers is needed for rising R -curve materials. Therefore, care should be taken in interpreting and utilizing fracture toughness values evaluated from different testing methods if a material exhibits a rising R -curve. Complete characterization of the R -curve may be a prerequisite.     

Foreign Object Damage Resistance of Silicon Nitride and Silicon Carbide

To clarify the foreign object damage (FOD) resistance of ceramics, chipping fracture mode and flexural fracture mode were investigated using several types of Si₃N₄ and Sic. The critical velocity which is the threshold impact velocity of the projectile for chipping fracture and flexural fracture was determined. The critical velocity of the chipping fracture mode is explained as a function of K ^5/2_IC a ^–5/4, and depends on the hardness and the shape of the projectile. The critical velocity of the flexural fracture mode is explained as a function of σ^5/6_C t ^5/3. The mechanisms of impact damage are discussed.     

In Situ Polysilane-Derived Silicon Carbide Particulates Dispersed in Silicon Nitride Composite

A dense (97% of theoretical density) Si₃N₄—SiC composite containing 10 wt%β-SiC was prepared by introducing a SiC phase by the pyrolysis of a polymeric SiC precursor. The composite material was produced by mixing an alkyl/aryl-substituted polysilane with Si₃N₄ powder and, by subsequently forming green compacts, pyrolyzing the polymeric species, and finally sintering the sample. Synthesis and characterization of the polymeric compound was described. Its transformation reactions to SiC and the characterization of the ceramic residue were also studied. High ceramic yields were obtained by curing the as-synthesized polysilane at 500°C in an Ar atmosphere. The heat treatment had no effect on the good solubility of the polymeric precursor in organic solvents. This was important for processes such as infiltration, sealing, and coating and for the mixing of the polymer with powders for the preparation of homogeneous composite ceramics. The dense microstructure of the pyrolyzed and sintered Si₃N₄ powder–polysilane mixture exhibited reduced grain growth of the Si₃N₄ particles and a very homogeneous distribution of the in situ-formed β-SiC phase.     

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.     

In Situ Synthesis of Silicon Carbide Whiskers from Silicon Nitride Powders

Silicon carbide whiskers were synthesized in situ by direct carbothermal reduction of silicon nitride with graphite in an argon atmosphere. Phase evolution study reveals that the formation of β-SiC was initiated at 1400° to 1450°C; above 1650°C silicon was formed when carbon was deficient. Nevertheless, Si₃N₄ could be completely converted to SiC with molar ratio Si₃N₄:C = 1:3 at 1650°C. The morphology of the SiC whiskers is needlelike, with lengths and diameters changing with temperature. SiC fibers were produced on the surface of the sample fired at 1550°C with an average diameter of 0.3 μm. No catalyst was used in the syntheses, which minimizes the amount of impurities in the final products. A reaction mechanism involving the decomposition of silicon nitride has been proposed.     

热压碳化硅耐磨复合材料的研究

采用热压法开发出SiCAl2O3和SiCAl2O3AlN系复合材料,并用其制成了石油产品输送泵端面密封装置,在使用条件下这种装置具有优良的物理机械性能。     

In Situ Processing of Silicon Carbide Layer Structures

A novel route to low-cost processing of silicon carbide (SiC) layer structures is desribed. The processing involves pressureless liquid-phase cosintering of compacted power layers of SiC, containing alumina (Al₂O₃) and yttria (Y₂O₃ sintering additives to yield and yttrium aluminum garnet (YAG) second phase. By adjusting the β:α SiC phase ratios in the individual starting powders, alternate layers with distinctively different microstructures are produced: (i) "homogeneous" microstructures, with fine equiaxed SiC grains, designed for high strength; and (ii) "heterogeneous: microstructures with coarse and elongate SiC grains, designed for high toughness. By virtue of the common SiC and YAG phases, the interlayer interfaces are chemically compatible and strongly bonded. Exploratory Hertzian indetation tests across a bilayer interface confirm the capacity of the tough heterogeneous layer to inhibit potentially dangerous cracks propagating through the homogeneous layer. The potential for application of this novel processing approach to other layer architectures and other ceramic systems is considered.     

In S/Yu-Toughened Silicon Carbide-Titanium Carbide Composites

A process based on liquid-phase sintering and subsequent annealing for grain growth is presented to obtain in situ -toughened SiC-30 wt% TiC composites. Its microstructures consist of uniformly distributed elongated α-SiC grains, matrixlike TiC grains, and yttrium aluminum garnet (YAG) as a grain boundary phase. The composites were fabricated from β-SiC and TiC powders with the liquid forming additives of A1₂O₃ and Y₂O₃ by hot pressing. During the subsequent heat treatment, the β→α phase transformation of SiC led to the in situ growth of elongated α-SiC grains. The fracture toughness of the SiC-30 wt% TiC composites after 6-h annealing was 6.9 MPa-m^1/2, approximately 60% higher than that of as-hot-pressed composites (4.4 MPa-m^1/2). Bridging and crack deflection by the elongated α-SiC grains appear to account for the increased toughness of this new class of composites.     

In Situ Toughened Silicon Carbide with Al-B-C Additions

" In situ toughened" silicon carbides, containing Al, B, and C additives, were prepared by hot pressing. Densification, phase transformations, and microstructural development were described. The microstructures, secondary phases, and grain boundaries were characterized using a range of analytical techniques including TEM, SEM, AES, and XRD. The modulus of rupture was determined from fourpoint bend tests, while the fracture toughness was derived either from bend tests of beam-shaped samples with a controlled surface flaw, or from standard disk-shaped compact-tension specimens precracked in cyclic fatigue. The R -curve behavior of an in situ toughened SiC was also examined. A steady-state toughness over 9 MPa·m^1/2 was recorded for the silicon carbide prepared with minimal additives under optimum processing conditions. This increase in fracture toughness, more than a factor of three compared to that of a commercial SiC, was achieved while maintaining a bend strength of 650 MPa. The mechanical properties were found to be related to a microstructure in which platelike grain development had been promoted and where crack bridging by intact grains was a principal source of toughening.     

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.     

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.     

Oxidation Resistance Evaluation of Silicon Carbide Ceramics with Various Additives

Five silicon carbide ceramics with various additives were evaluated for oxidation resistance at 1300°C in flowing dry and wet air. In the dry atmosphere, the oxidation of the five samples was diffusion-controlled, and in wet atmosphere they exhibited a linear relation beween weight gain by oxidation and water vapor content. Water vapor in the atmosphere strongly accelerated oxidation. The influence of oxidation on room-temperature strength was complex, but the samples were not as affected by oxidation.     

Oxidation Resistance of Multiwalled Carbon Nanotubes Coated with Silicon Carbide

Multiwalled carbon nanotubes (MWCNTs) were coated with a SiC layer using SiO vapor. The growth mechanism of SiC and the oxidation resistance of the SiC-coated MWCNTs were studied. The growth of the SiC layer was controlled by adjusting the partial pressure of CO₂ using carbon felt placed in a crucible. The nanometer-sized SiC particles were deposited onto the tubes by the reaction between SiO( g ) and CO( g ). On the other hand, the thin surface of the MWCNTs was converted to the SiC layer when the carbon felt was not used. The oxidation durability of MWCNTs was improved by the SiC coating. MWCNTs were oxidized completely in air at 650°C for 60 min. However, about 90 mass% of the SiC-coated MWCNTs remained after the same oxidation test.     

Steam Oxidation Resistance of Silicon Carbide Castables at Elevated Temperatures

Silicon carbide castables of different SiC contents (86％ and 71％,by mass) were prepared using white fused corundum,silicon carbide particles and fines,activated...     

A Constitutive Model for In Situ Comminuted Silicon Carbide

Cylindrical hot-pressed silicon carbide (SiC) ceramic targets were predamaged before ballistic testing. The SiC was thermally shocked to introduce noncontiguous cracks, then additional damage was induced by load–unload cycling in an MTS machine while the ceramic specimen was confined in a 7075-T6 aluminum sleeve. Long gold rod penetration was measured as a function of impact velocity v _p over the approximate range of 1–3 km/s, with most data between 1.5 and 3 km/s. Penetration as a function of time was measured using multiple, independently timed flash X-rays. It was assumed that the penetration response of the damaged SiC could be represented by a Drucker–Prager constitutive model. Numerical simulations were used to estimate the constitutive constants. It was found that simulations could not be used to determine a unique set of constitutive constants within experimental data scatter.     

In Situ Gas–Solid Reaction and Oxidation Resistance of Silicon Carbide Coating on Carbon Fibers

Silicon carbide (SiC) coating on carbon fibers was realized based on in situ low‐temperature gas–solid reaction processing in which carbon reacted with Si vapor at the temperature of 1200°C–1300°C. X‐ray diffraction (XRD), field‐emission scanning electron microscopy (FE‐SEM), and energy‐dispersive spectroscopy (EDS) analysis showed that the SiC coating was uniform and crystallized by beta‐SiC. The oxidation resistant properties of the SiC‐coated carbon fibers were significantly improved according to isothermal oxidation measurement. The initial oxidation temperature of the SiC‐coated carbon fibers was about 200°C higher than that of the raw carbon fibers. The SiC‐coating carbon fibers treated at 1250°C possessed higher antioxidant property than the one treated at 1300°C.     

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.