Microstructure and Reactions of SiCw-Reinforced Alumina with Ag-Cu-In-Ti

Brazing experiments were performed at 750°C for 2 h between Ag–Cu–In–Ti alloy and SiC_w/Al₂O₃. The first clearly nonbraze layer consists of an oxide layer of metallic composition 33Ti–31Al–22Cu–14Si. Areas adjacent to the SiC whiskers were of different composition. A thin, continuous layer on the alumina portion of the composite appears to be γ-TiO. The SiC whiskers are preferentially consumed and undergo reductions in diameter of approximately 40%. Observed "knobby" whisker morphologies may be related to SiC stacking faults, η-type phases detected near the Ag–Cu eutectic portion of the joint appear to consist of Ti-Cu-Al-Si-O and Ti₃Cu₃O.     

Behavior of Cyclic Fatigue Cracks in Monolithic Silicon Nitride

Cyclic fatigue-crack propagation behavior in monolithic silicon nitride is characterized in light of current fatiguecrack growth models for ceramics toughened by grainbridging mechanisms, with specific emphasis on the role of load ratio. Such models are based on diminished cracktip shielding in the crack wake under cyclic loads due to frictional-wear degradation of the grain-bridging zone. The notion of cyclic crack growth promoted by diminished shielding is seen to be consistent with measured (long-crack) growth rates, fractography, in situ crack-profile analyses, and measurements of back-face strain compliance. Growth rates are found to display a much larger dependence on the maximum applied stress intensity, K _max than on the applied stress-intensity range, Δ K , with behavior described by the relationship da/dN ∞ K²⁹_maxΔK^1.3. Fatigue thresholds similarly exhibit a marked dependence on the load ratio, R = K _min/ K _max; such effects are shown to be inconsistent with traditional models of fatigue-crack closure. In particular, when characterized in terms of K _max growth rates below ∼10⁻⁹ m/cycle exhibit an inverse dependence on load ratio, an observation which is consistent with the grain-bridging phenomenon; specifically, with increasing R, the sliding disance between the grain bridges is decreased, leading to less frictional wear, and hence less degradation in shielding, per loading cycle. The microstructural origins of such behavior are discussed.     

Stable Crack Growth in Polycrystalline Magnesia under Monotonic and Cyclic Loads

The quasi-static, stable growth of cracks in polycrystalline magnesia under various loading conditions (cyclic compression, monotonic tension, and tension–compression fatigue) was studied. Crack length was monitored continuously through a conductive film attached to the specimen surface. The fracture surfaces and the crack path were examined by scanning electron microscopy. The different fracture mechanisms responsible for the observed stable crack growth in each loading condition are discussed.     

Evaluation of Whisker Alignment in Axisymmetric SiCw-Reinforced Al2O3 Composite Material

A quantitative method to evaluate the degree of whisker alignment in axisymmetric composite materials was developed. The angular distribution of the whiskers was analyzed by measuring the aspect ratios of the whiskers observed on a planar section. However, due to the large difference in the probability of whiskers being detected on the planar section (depending on whisker length and degree of alignment), the angular distribution of the whiskers observed on the planar section was significantly different from the actual distributions of the whiskers in three dimensions. Three-dimensional angular distributions were evaluated by comparing the aspect ratios observed on the planar section with those calculated under the assumption that the whisker angle fell in a Gaussian distribution with average angle of 90°. By this method, the degree of preferential alignment is expressed as the standard deviation of the Gaussian distribution. This quantification of whisker alignment is useful in analyzing the mechanical behaviors of composite materials reinforced with elongated particles.     

Mechanical and Environmental Factors in the Cyclic and Static Fatigue of Silicon Nitride

The effects of environment on cyclic and static fatigue behavior were investigated with hot-pressed silicon nitride materials. Tests were conducted at ambient temperature on standard compact tension specimens, and a dc electric potential technique was used to monitor crack lengths in situ. The results indicate that the environmental sensitivity of our materials under both cyclic and static loading mirrors that of durable glasses in static fatigue. The materials were most sensitive to water in the environment, while changes in pH had no significant effect in the range tested. In addition, NH₃ was much less reactive with our materials than with vitreous SiO₂. In some cases, the intergranular glass appears to be the site of environmental interaction. Evidence was also found that cyclic fatigue is not simply a manifestation of static fatigue. Cyclic fatigue was seen to occur in the absence of measurable static fatigue, and the data indicate that the mechanism of cyclic fatigue involves damage to the crack wake shielding zone.     

Crack Deflection and Propagation in Layered Silicon Nitride/Boron Nitride Ceramics

Crack deflection and the subsequent growth of delamination cracks can be a potent source of energy dissipation during the fracture of layered ceramics. In this study, multilayered ceramics that consist of silicon nitride (Si₃N₄) layers separated by boron nitride/silicon nitride (BN/Si₃N₄) interphases have been manufactured and tested. Flexural tests reveal that the crack path is dependent on the composition of the interphase between the Si₃N₄ layers. Experimental measurements of interfacial fracture resistance and frictional sliding resistance show that both quantities increase as the Si₃N₄ content in the interphase increases. However, contrary to existing theories, high energy-absorption capacity has not been realized in materials that exhibit crack deflection but also have moderately high interfacial fracture resistance. Significant energy absorption has been measured only in materials with very low interfacial fracture resistance values. A method of predicting the critical value of the interfacial fracture resistance necessary to ensure a high energy-absorption capacity is presented.     

Mechanical Properties of Three-Layered Monolithic Silicon Nitride–Fibrous Silicon Nitride/Boron Nitride Monolith

A three-layered composite, composed of a strong outer layer (monolithic S₃N₄) and a tough inner layer (fibrous Si₃N₄/BN monolith), was fabricated by hot-pressing. For the inner layer, a Si₃N₄–polymer fiber made by extrusion was coated by dipping it into a 20 wt% BN-containing slurry. The three-layered composite exhibited excellent mechanical properties, including high strength, work of fracture, and crack resistance, because of the combination of a strong outer layer and a tough inner layer. In other words, the strong outer layer withheld the applied stress, while the tough inner layer promoted crack interactions through the weak BN cell boundaries. Also, the residual thermal stress on the surface due to the anisotropy in the coefficient of thermal expansion of BN affected a median/radial crack generation after indentation.     

Dynamics of Consolidation and Crack Growth in Nanocluster-Assembled Amorphous Silicon Nitride

Consolidation and fracture dynamics in nanophase amorphous Si3N4 are investigated using 106-atom molecular-dynamics simulations. At a pressure of 15 GPa and 2000 K, the nanophase system is almost fully consolidated within a fraction of a nanosecond. The consolidation process is well-described by the classical theory of sintering. Under an applied strain the consolidated system develops several cracks which propagate parallel to each other, causing failure at multiple sites. The critical strain at which the nanophase system fractures is much larger than that for crystalline Si3N4.     

Elevated-Temperature Mechanical Properties of Silicon Nitride/Boron Nitride Fibrous Monolithic Ceramics

A unique, all-ceramic material capable of nonbrittle fracture via crack deflection and delamination has been mechanically characterized from 25° through 1400°C. This material, fibrous monoliths, was comprised of unidirectionally aligned 250 μm diameter silicon nitride cells surrounded by 10 to 20 μm thick boron nitride cell boundaries. The average flexure strengths of fibrous monoliths were 510 and 290 MPa for specimens tested at room temperature and 1300°C, respectively. Crack deflection in the BN cell boundaries was observed at all temperatures. Characteristic flexural responses were observed at temperatures between 25° and 1400°C. Changes in the flexural response at different temperatures were attributed to changes in the physical properties of either the silicon nitride cells or boron nitride cell boundary.     

Subcritical Crack Growth in Sintered Silicon Nitride Exhibiting a Rising R-Curve

Subscritical crack growth of sintered silicon nitride was analyzed in terms of the R -curve. Provided that the stress intensity at the crack tip governs the subcritical crack-growth velocity, the K _I– V relationship of sintered silicon nitride exhibiting a rising R -curve is shown to shift to the high- K _I region as the crack advances.     

Static and Cyclic Fatigue Behavior of a Sintered Silicon Nitride at Room Temperature

The static and cyclic fatigue behavior of sintered silicon nitride was investigated at room temperature. Flexure specimens, with an indentation-induced flaw at the center, were tested under a static or cyclic load applied by four-point bending. Sintered silicon nitride was shown to be susceptible to static and cyclic fatigue failure. Comparing the static and cyclic fatigue lifetimes at frequencies from 0.01 to 10 H z , it was shown that minimum time to failure was almost the same, in spite of differences in loading mode or frequency. However, cyclic stress decreased the scatter in lifetime by reducing the upper limit. Moreover, the cyclic fatigue limit was significantly lower than the static fatigue limit. High-magnification fractography revealed a fatigue failure dominated by intergranular cracking with partial transgranular failure at perpendicularly elongated crystals. This suggests that the intergranular fatigue crack can be arrested at grain-boundary triplets, and also can be reactivated by subsequent cyclic loading. The crack growth rate, calculated from the fatigue lifetime, showed three characteristic regions having a plateau at 70% to 90% of the fracture toughness, which suggests a possible intergranular stress corrosion cracking mechanism resembling that in glass or alumina.     

Comparison of High-Temperature Crack Growth in SiC-Whisker-Reinforced Mullite and Si3N4

Crack growth behavior under creep conditions was studied in SiC-whisker-reinforced mullite and silicon nitride. Tests of four-point bend specimens with indentation cracks were periodically interrupted to observe the creep behavior. At each interruption the bulk creep strain of the specimen, the growth of the indentation cracks, and the nucleation and growth of creep-induced cracks were measured. A strong linear correlation was observed in both materials between the crack growth rate and the creep strain rate. For a given strain rate, cracks in the silicon nitride composite propagated at velocities about an order of magnitude greater than those in the mullite composite. On the other hand, for similar nominal stresses, creep rates in the silicon nitride composites were about an order of magnitude less than with the mullite composite.     

Studies on Abrasive Wear of Monolithic Silicon Nitride and a Silicon Carbide Whisker-Reinforced Silicon Nitride Composite

Results presented in this paper demonstrate the roles of the most important parameters that govern abrasive wear of experimental ceramics. SEM studies of the abraded surfaces evidenced two main kinds of failures: microdropping of grain(s) and powder-type wear track(s) resulting from the brittle microfracturing of parts of grain(s). There were whiskers in the surface, and whisker pullouts occurring during wear processes are believed to be the reasons for the lower wear rates of SiCw/Si₃N₄ composite ceramics under experimental conditions.     

Spark-Plasma Sintering of Silicon Carbide Whiskers (SiCw) Reinforced Nanocrystalline Alumina

The combined effect of rapid sintering by spark-plasma-sintering (SPS) technique and mechanical milling of γ-Al₂O₃ nanopowder via high-energy ball milling (HEBM) on the microstructural development and mechanical properties of nanocrystalline alumina matrix composites toughened by 20 vol% silicon carbide whiskers was investigated. SiC_w/γ-Al₂O₃ nanopowders processed by HEBM can be successfully consolidated to full density by SPS at a temperature as low as 1125°C and still retain a near-nanocrystalline matrix grain size (∼118 nm). However, to densify the same nanopowder mixture to full density without the benefit of HEBM procedure, the required temperature for sintering was higher than 1200°C, where one encountered excessive grain growth. X-ray diffraction (XRD) and scanning electron microscopy (SEM) results indicated that HEBM did not lead to the transformation of γ-Al₂O₃ to α-Al₂O₃ of the starting powder but rather induced possible residual stress that enhances the densification at lower temperatures. The SiC_w/HEBMγ-Al₂O₃ nanocomposite with grain size of 118 nm has attractive mechanical properties, i.e., Vickers hardness of 26.1 GPa and fracture toughness of 6.2 MPa·m^1/2.     

Crack Healing in a Silicon Nitride Ceramic

A detailed study has been undertaken on crack healing at high temperatures in a silicon nitride containing 10 wt% additives in order to identify the dominant mechanism responsible for the phenomenon. Fracture toughness increased with annealing time and the crack growth rate decreased until arrest with increasing testing time. Differentiation between possible operating mechanisms was obtained using critical experiments involving detailed compliance measurements, crack wake removal, and crack reinitiation tests and a comprehensive TEM study of healed cracks. It was found that crack healing was not uniform in the crack wake. When the original crack path was either transgranular or intergranular, healing was associated with the appearance of a thin layer of silica glass due to the oxidation of Si₃N₄ grains. But when the crack went through multigrain junctions, the former crack path was completely obliterated and replaced by a new, crystalline phase formed by diffusion of the preexisting glass phase. It is concluded that the increased crack growth resistance and fracture toughness at high temperature is attributable to the partial recovery of the original strength from the crack segments at multigrain junctions due to vitreous phase flow and subsequent crystallization.     

Crack Propagation Behavior of Polycrystalline Alumina under Static and Cyclic Load

Various causes for cyclic-loading fatigue in ceramics have been proposed. Degradation in the grain-bridging effect is the most important cause for cyclic-loading fatigue in nontransforming ceramics. Cyclic- and static-loading crack propagation behavior in terms of crack propagation rate, load—strain curve, and R -curve in compact tension specimens of polycrysalline aluminas with two types of average grain size is reported. Significant bridging is observed in coarse-grained alumina. The results are consistent with the proposal that grain bridging increases with grain size and that degradation in grain bridging is the most important cause for cyclic-loading fatigue in alumina ceramics.     

High-Temperature Toughness and Tensile Strength of Whisker-Reinforced Silicon Nitride

The R -curve behavior of hot-pressed silicon nitride reinforced with silicon carbide whiskers is investigated from room temperature to 1300°C using the chevron-notch bend test. The bridging stress, estimated from increment of fracture resistance in the rising R -curve, is discussed in relation to tensile strength measured with various displacement rates at 1300°C. The reinforcing whiskers provide most of the tensile strength in the creep-deformation range at 1300°C. The whiskers appear to bear a great deal of the applied tensile stress during slow crack growth.     

Fracture of Si3N4–SiC Whisker Composites under Cyclic Loads

This communication demonstrates the role of cyclic compressive loads in inducing mode I fatigue crack growth at room temperature in Si₃N₄ matrix–SiC whisker composite materials containing stress concentrations. The characteristics of stable, cyclic fracture are examined for several volume fractions of the SiC whisker and are compared with those of the matrix material. It is found that the composites with higher volume fractions of SiC whiskers exhibit an inferior resistance to fracture under cyclic compressive loads despite improvements in fracture toughness values.     

High-Temperature Strength Behavior of Hot-Pressed Si3N4: Evidence for Subcritical Crack Growth

The high-temperature strength of commercial hot-pressed Si₃N₄ was obtained for (1) two materials with different impurity contents, (2) the weak and strong material directions, (3) air and Ar ambients, and (4) different stressing rates. Strength degradation occurred at a lower temperature for the less pure material; both material directions exhibit the same rate of strength degradation. The testing ambient did not affect strength. The strength at temperatures ∼1200°C depended strongly on stressing rate. The presence of rough, crack-shaped topographical features on the fracture surface and the observation of large cracks that formed during stressing are reported as evidence for subcritical crack growth at high temperatures. It is hypothesized that accelerated creep caused by grain-boundary sliding at preexisting crack fronts is the mechanism responsible for the observed subcritical crack growth.