Fatigue Threshold R‐curves Predict Fatigue Endurance Strength for Self‐Reinforced Silicon Nitride

There is a need for methods that can help predict and avoid fatigue failures of silicon nitride ceramic components. The fatigue threshold R‐curve has been proposed as potential solution to this problem. In this study, the fatigue threshold R‐curve for small, semielliptical surface cracks was calculated for a silicon nitride ceramic using the published bridging stress distribution developed from fatigue threshold tests on macroscopic crack specimens. To test the accuracy of the endurance strengths predicted using the fatigue threshold R‐curve, fatigue tests were conducted using four‐point bend beams of silicon nitride containing semielliptical surface cracks introduced by Knoop indentation. The effectiveness of the methodology was verified; indeed, 77% of the beams tested at stress levels above the predicted endurance strength failed within 10⁷ cycles and 0% of the beams tested below the predicted endurance strength failed within 10⁷ cycles. Furthermore, using the bridging stress distribution, which is thought to be a material property, the need for prohibitively difficult fatigue threshold experiments on small surface cracks is avoided. Accordingly, this methodology is potentially quite practical for use in the engineering design of ceramic mechanical components.     

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.     

Fatigue Crack Growth of Silicon Nitride at 1400°C: A Novel Fatigue-Induced Crack-Tip Bridging Phenomenon

high-strength Si₃N₄with elongated β-Si₃N₄ and equiaxed α-sialon was tested in cyclic and static fatigue at 1400°C. At low stress intensity factors and high frequencies, the pullout process of the elongated grains was enhanced, which suppressed the crack growth. This provides a possible explanation for the increased lifetime under cyclic leading conditions reported for ceramics by several investigators. While crack-healing by high-temperature annealing was found to greatly reduce the subsequent static fatigue crack growth rate, it had only a modest effecf on cyclic fatigue and none at high frequencies.     

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.     

Fatigue Crack Growth Behavior of Silicon Nitride: Roles of Grain Aspect Ratio and Intergranular Film Composition

The role of microstructure in affecting the fatigue crack growth resistance of grain bridging silicon nitride ceramics doped with rare earth (RE = Y, La, Lu) oxide sintering additives was investigated. Three silicon nitride ceramics were prepared using MgO‐RE₂O₃ and results were compared with a commercial Al₂O₃‐Y₂O₃‐doped material. Decreasing stress intensity range (ΔK) fatigue tests were conducted using compact‐tension specimens to measure steady‐state fatigue crack growth rates. Specimens doped with MgO‐RE₂O₃ additives showed a significantly higher resistance to crack growth than those with Al₂O₃‐Y₂O₃ additives and this difference was attributed to the much higher grain aspect ratio for the MgO‐RE₂O₃‐doped ceramics. When the crack growth data were normalized with respect to the total contribution of toughening by bridging determined from the monotonically loaded R‐curves, the differences in fatigue resistance were greatly reduced with the data overlapping considerably. Finally, all of the MgO‐RE₂O₃‐doped silicon nitrides displayed similar steady‐state fatigue crack growth behavior suggesting that they are relatively insensitive to the intergranular film.     

Model for Fatigue Crack Growth in Grain-Bridging Ceramics

A model for fatigue crack propagation based on sliding wear of bridging grains is analyzed for polycrystalline ceramics. Taking into account damage development and crack tip energy balance, we have obtained rigorous solutions for equilibrium and compatibility equations in the crack wake under monotonic and cyclic loading/unloading conditions. Fatigue mechanics in ceramics is found to be formally similar to elastic-plastic mechanics of a path-dependent hardening material, due to the frictional resistance to reverse sliding. It features a load-displacement hysteresis causing energy dissipation and wear, and a longer cohesive zone required for supporting the same peak load with the wear-reduced bridging stresses. The unloading crack opening displacement is more strongly dependent on K _max than on Delta K ; such displacement causes wear on the bridging grains. Meanwhile, incremental crack growth brings in new bridging grains that has a shielding effect on the crack tip stress field; such an effect is strongly dependent on K _max but independent of Delta K . At steady state, when shielding accumulation and shielding degradation are balanced, the fatigue crack growth rate has a form d a /d N = A ( K _max) ^b (Delta K ) ^c , where A, b , and c are material-dependent parameters. Fatigue is predicted to have a very high b , a modest c , a higher fatigue resistance for tougher ceramics, and a stronger K _max dependence for less tough ceramics. These predictions are in agreement with experimental observations.     

Fracture Resistance Behavior of High‐Thermal‐Conductivity Silicon Nitride Ceramics

Silicon nitride ceramics were prepared from a high‐purity silicon powder doped with 2 mol% Y₂O₃ and 5 mol% MgO as sintering additives via a route of sintering of reaction‐bonded silicon nitride (SRBSN). The materials sintered at 1900°C for 3, 6, 12, and 24 h had thermal conductivities of 109, 125, 146, and 154 W/m/K, and four‐point bending strengths of 786, 676, 608, and 505 MPa, respectively. The fracture toughness values, determined by the single‐edge‐precracked‐beam (SEPB) method, were 8.4, 8.6, 9.7, and 10.7 MPa m^1/2 for the materials sintered for 3, 6, 12, and 24 h, respectively, which were similar to the results measured by the chevron‐notched‐beam (CNB) test method. The materials sintered for longer times (12 and 24 h) showed stronger R‐curve behaviors over longer range of crack extension, in comparison with the materials sintered for shorter times (3 and 6 h).     

Elevated-Temperature Creep of Silicon Carbide-Aluminum Nitride Ceramics: Role of Grain Size

Samples containing 50 mol% SiC and 50 mol% AIN were fabricated to neartheoretical density by hot-pressing in graphite dies in N₂ atmosphere. Grain size was varied by varying the hot-pressing conditions. Bar-shaped samples cut from the billets were subjected to creep deformation in four-point bending. Creep was found to depend upon the grain size with coarse-grained material exhibiting lower creep rate. The stress exponent was ∼2.0.     

Sintering of High‐Performance Silicon Nitride Ceramics Under Vibratory Pressure

To improve mechanical behaviors of silicon nitride ceramics, here we introduced a novel external field—vibratory pressure into the sintering of Si₃N₄ ceramics with advantages of higher density, more uniform distribution of interfacial phase, higher sintering motivation in the width direction, and therefore more favorable mechanical properties than traditional sintering methods. Grain size and aspect ratio of the two ceramics were investigated with linear intercept method. Flexural strength of the vibratory‐assisted hot‐pressing (VAHP) specimen increased from 936 ± 27.2 MPa to 1247 ± 28.9 MPa, and an increase of 10% was achieved in fracture toughness. It is believed that such VAHP method can provide a universal approach and new opportunities for the fabrication of covalent‐bonded ceramics or composites with enhanced performances.     

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.     

Threshold Stress Intensity for Crack Growth in Silicon Carbide Ceramics

Measurements of threshold stress intensities for crack growth, K _h, of three polycrystalline SiC materials were attempted using interrupted static fatigue tests at 1200°–1400°C. Weibull statistics were used to calculate conservative K_th values from test results. The K _th of a chemically vapor deposited β-SiC could not be determined, as a result of its wide variations in strength. The K_th ≥ 3.3,2.2, and 1.7 MPa·m^1/2 for an Al-doped sintered α-SiC; and K_th ≥ 3.1, 2.7, and 2.2 MPa·m^1/2 for a hot isostatically pressed α-SiC, both at 1200°, 1300°, and 1400°C, respectively. A damage process concurrent with subcritical crack growth was apparent for the sintered SiC at 1400°C. The larger K_th 's for the HIPed SiC (compared to the sintered SiC) may be a result of enhanced viscous stress relaxation caused by the higher silica content and smaller grain size of this material. Values measured at 1300° and 1400°C were in good agreement with the K_th's predicted by a diffusive crack growth model, while the measured K_th 's were greater than the predicted ones at 1200°C.     

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.     

Fatigue Crack Growth from Small Surface Cracks in Transformation-Toughened Ceramics

A theoretical model based on the theory of complex potentials and dislocation formalism is used to simulate the fatigue crack growth of small cracks in a transformation-toughened ceramic. Assuming power-law crack growth in which the growth rate depends on the effective stress intensity at the crack tip instead of the applied stress intensity, it is shown that the crack growth rate decreases with the applied stress intensity in the initial stage of fatigue crack growth. This is in agreement with existing experimental evidence for the growth of small cracks in Mg-PSZ. New experimental results obtained by in situ observation in a scanning electron microscope of a similar material confirm this behavior. The numerical results also confirm the plausibility of using the steady-state toughness value obtained from quasi-static crack growth as a normalizing parameter in the power-law for fatigue crack growth.     

Silicon Nitride Ceramics Prepared by Vibratory Casting of Self-Reinforced Mixtures: Testing for Crack Resistance

Technological factors capable of influencing the structure, physicomechanical properties, and crack resistance of silicon nitride ceramics intended for fabrication of component of complex shape are considered. The effect of a composite sintering aid Al₂O₃ + Y₂O₃ and an ethyl silicate binder on strength and crack resistance of raw and sintered ceramics subjected to hydrostatic compression is discussed. It is shown that the ceramics in question can be tested for crack resistance by the indentation method.     

Oxidation Behavior of Rare-Earth Disilicate–Silicon Nitride Ceramics

The oxidation behavior and microstructure of the oxidized surfaces of RE₂Si₂O₇–Si₃N₄ ceramics were investigated. The high oxidation resistance of these materials at 1400°C is attributed to the minimization of amorphous phases via devitrification to disilicates that are in equilibrium with SiO₂, the oxidation product of Si₃N₄. Crystals of RE₂Si₂O₇ grew out of the surface silicate in prefered orientations that were dictated by crystal structure. The morphology of the microstructure of the oxidized surfaces was shown to be partially dependent on the concentration of impurities; the presence of Ca was found to coincide with the growth of Gd₂Si₂O₇ and Dy₂Si₂O₇ crystals with high aspect ratios.     

Retardation of Fatigue Crack Growth in Ceramics by Glassy Ligaments: A Rationalization

In high-temperature fatigue crack growth (FCG) experiments on ceramic materials containing amorphous grain boundary phases, the crack growth rates under cyclic loads were observed to be lower than those predicted solely on the basis of crack growth velocities measured under static loads. In this paper, a rationalization was offered for such a behavior by means of a phenomenological glass-bridging model which takes the relaxation behavior of glass into account. In ceramics which exhibit subcritical crack growth through cavitation ahead of the crack tip, the maximum stress intensity factor of the fatigue cycle required to initiate FCG was observed to be always greater than or equal to the threshold stress intensity factor for crack growth under sustained far-field loads. This trend was also explained with the aid of the glass-bridging model and invoking the equivalence between bridging and damage zones. The elevated temperature FCG behavior of nitride-based ceramics which exhibit grain bridging in the wake during crack propagation was discussed and contrasted with oxide-based ceramics which show glass bridging.     

Preparation of β-Silicon Nitride Seeds for Self-Reinforced Silicon Nitride Ceramics

This paper describes a method for the preparation of silicon nitride (Si₃N₄) seeds that have an average aspect ratio of ∼4. The seeds are prepared via heat treatment of a powder mixture that contains alpha-phase-rich Si₃N₄ and 0.5 wt% Y₂O₃ at a temperature of 1800°C and a nitrogen pressure of 35 kPa. A Y-Si-O-N liquid forms during heat treatment; this liquid acts as a flux for seed precipitation. During cooling, the Y-Si-O-N liquid transforms to a thin intergranular grain-boundary phase and causes strong agglomeration of the seeds. The seeds can be isolated by dissolving the grain-boundary phase in hot phosphoric acid, followed by an ultrasonic treatment (for 30 min). The method can be used to produce large quantities of seeds.     

Relation Between Multiregion Crack Growth and Dynamic Fatigue of Glass Using Indentation Flaws

The influence of transport-limited kinetic crack growth on the fatigue properties of soda-lime glass was examined. Dynamic fatigue data were taken on specimens with controlled indentation flaws and were compared with the predicted response from measured crack velocity characteristics. Heptane was used as the operational test environment because of its pronounced crack velocity plateau; control tests in water served to establish a baseline reference for comparing the results. Frac-tographic observations using a stress wave marker technique showed a complex growth history for flaws broken in heptane compared to that for flaws broken in water. The magnitude of the predicted region II influence is too small to be detected in the dynamic fatigue results, even allowing for the relatively high degree of data reproducibility. The implications of this conclusion for lifetime predictions are discussed.     

Fatigue Crack Growth in Ferroelectric Ceramics Driven by Alternating Electric Fields

Electric-field-induced fatigue crack growth in ferroelectric ceramic PZT-5 with precracks was investigated. The experimental results showed that there were two distinct characteristics in the crack growth under electric loading. Under low electric loads, microcracks located ahead of the main crack emerged and grew and, as a result, impeded the growth of the main crack. On the other hand, under high electric loads, microcracks were absent, and the main crack was the only mode of fatigue cracking. The main crack grew macroscopically along the original path perpendicular to the electric field. Microscopically, the crack grew along the grain boundaries and grain breakaway was observed. The crack growth rate was nonlinearly related to the cyclic electric load. Similar to mechanical fatigue, there existed a crack growth threshold in the applied electric-field amplitude below which the crack ceased to grow. A steady crack growth occurred when the applied electric field exceeded this threshold. An empirical model for crack growth was obtained. Domain-switching effect and fracture-mechanics concepts were used to explain the observed crack closure and crack growth under electric loads.