Fracture Toughness and Thermal Shock Behavior of Silicon Nitride–Boron Nitride Ceramics

Fracture toughness behavior, stress–strain behavior, and flaw resistance of pressureless-sintered Si₃N₄-BN ceramics are investigated. The results are discussed with respect to the reported thermal shock behavior of these composites. Although the materials behave linear-elastic and exhibit no R -curve behavior, their flaw resistance is different from that of other linear-elastic materials. Whereas the critical thermal shock temperature difference (Δ T _c) is enhanced by adding BN, the content of BN has no influence on the strength loss during severe thermal shocks.     

R-Curve Behavior in a Silicon Carbide Whisker/Alumina Matrix Composite

R -curve measurements were performed on a SiC whisker/Al₂O₃ matrix composite. A controlled flaw/strength technique was utilized to determine fracture resistance as a function of crack extension. Rising R -curve behavior with increasing crack extension was observed, confirming the operation of wake toughening effects on the crack growth resistance. Observations of crack/microstructure interactions revealed that bridging by intact whiskers in the crack wake was the mechanism responsible for the rising R -curve behavior.     

Fracture Resistance of a Transparent Magnesium Aluminate Spinel

The fracture resistance of a fully dense, transparent, polycrystalline magnesium aluminate spinel was measured from room temperature to 1400°C using the chevron-notched beam and the straight-notched beam macroflaw techniques, as well as the indentation-induced, controlled-microflaw test method, all in three-point bending. Flexural strengths were also measured for the same range of temperatures to compare with the fracture toughness measurements. From the load vs load-line displacement ( P-u ) curves of the chevronnotched test specimens, the crack growth resistance curves ( R -curves) and the total work-of-fracture were determined. It was observed that polycrystalline MgAl₂O₄ exhibits rising R -curve behavior which increases with increasing test temperature. The R -curve increases are attributed to the geometric constraints due to grain bridging and grain wedging phenomena as well as secondary grain boundary microcracking processes, all of which occurred in the wake region behind the advancing crack. The work-of-fracture and the R -curves increased rapidly above 800°C coincident with the onset of increased secondary grain boundary microcracking.     

R-Curve Behavior and Flaw Insensitivity of Ce-TZP/Al2O3 Composite

A ceria-partially-stabilized zirconia-aiumina (Ce-TZP/Al₂O₃) composite optimized for transformation toughening was used to demonstrate its flaw insensitivity due to R -curve behavior. Four-point bend specimens fabricated with a controlled distribution of spherical pores showed nearly the same characteristic strength and strength variability (Weibull modulus) as specimens fabricated without the artificial pores. In situ observations confirmed stable growth of cracks initiated at pores and the crack lengths at fracture instability were much greater than the pore sizes, thus resulting in fracture strengths insensitive to the pores. The small variability in the fracture strength was found to be associated with variability in the R -curve and the instability crack lengths. An analysis based on the fracture instability criterion for rising crack growth resistance accounted for the strength variability due to variability in the R -curve. Comparable four-point bend experiments were also conducted on a sintered yttria-partially-stabilized zirconia (2Y-TZP) ceramic. This ceramic showed significant degradation of strength due to the presence of the pores. This flaw sensitivity is attributed to its steep rising R -curve over short crack lengths.     

The Utility of R-Curves for Understanding Fracture Toughness-Strength Relations in Bridging Ceramics

The mechanical behavior of four rare earth (RE)-Mg-doped Si₃N₄ ceramics (RE=La, Lu, Y, Yb) with varying grain-boundary adhesion has been examined with emphasis on materials containing La and Lu (which represent the extremes of RE ionic radius). Fracture-resistance curves ( R -curves) for all ceramics rose very steeply initially, giving them exceptional strength and relative insensitivity to flaw size. The highest strength was seen in the Lu-doped material, which may be explained by its steeper initial R -curve; the highest "apparent" toughness (for fracture from millimeter-scale micronotches) was seen in the lowest strength La-doped material, which may be explained by its slowly rising R -curve at longer crack lengths. Excellent agreement was found between the predicted strengths from R -curves and the actual strengths for failures originating from natural flaws, a result attributed to careful estimation of the early part of the R -curve by deducing the intrinsic toughness, K ₀, and the fact that this portion of the R -curve is relatively insensitive to sample geometry. Finally, it was found that RE elements with relatively large ionic radius (e.g., La) tended to result in lower grain-boundary adhesion. This implies that there is a small window of optimal grain-boundary adhesion which can lead to the fastest rising R -curves (for short cracks) and the highest strengths. The importance of this work is that it reinforces the notion that factors which contribute to the early part of the R -curve are critical for the design of ceramic microstructures with both high strength and high toughness.     

Toughening Behavior of a Two-Dimensional SiC/SiC Woven Composite at Ambient Temperature: I, Damage Initiation and R-Curve Behavior

The damage initiation and R -curve behavior for a two-dimensional (2-D) SiC/SiC woven composite are characterized at ambient temperature and related to in situ microscopic observations of damage accumulation and crack advance. Matrix cracking and crack deflection/branching are observed and dominate fracture behavior in the early loading stage such that primary crack extension occurs at apparent stress intensity values as high as 12 MPam^1/2. Linear elastic fracture mechanics (LEFM), though questionable, was assumed to be valid in the early stages of damage initiation prior to primary crack advance, but was clearly invalid once primary crack extension had occurred. Such a high primary crack extension toughness value is confirmed by a renotch technique whereby the crack wake is removed and the fracture resistance drops close to the initial value. Based on microstructural observations, multiple matrix cracks are found to be arrested at fiber bundles. The key to toughening appears to be associated with the mechanics of crack arrest at fiber bundles in the woven architecture. Toughening mechanisms include multiple matrix cracking (similar to microcracking), crack branching, and crack deflection in the crack frontal zone. Application of models to evaluate toughening based on these mechanisms results in values comparable to experimental data. In the regime of primary crack extension, a J -integral technique was applied to investigate the R -curve behavior and results showed a rising J_R -curve which started at 1500 J/m² and reached 6150 J/m² after about 13 mm of primary crack extension. There was evidence of substantial crack bridging by fiber tows and fibrous pull-out in this regime of crack advance.     

Flaw-Tolerance and R-Curve Behavior of Liquid-Phase-Sintered Silicon Carbides with Different Microstructures

β-SiC powder containing 6 wt% A1₂O₃ and 4 wt% Y₂O₃ as sintering additives was pressureless sintered at 2000°C for 1 h (AYE-SiC) and 3 h (AYP-SiC). AYE-SiC consisted of an equiaxed grain structure and AYP-SiC exhibited a micro-structure with platelike grains as a result of grain growth related to β→α phase transformation during sintering, R -curve behavior and flaw tolerance for these silicon carbides were evaluated by the indentation-strength technique. For comparison, the R -curve behavior of conventional sintered, boron- and carbon-doped SiC (SS-SiC) was evaluated. AYE-SiC and AYP-SiC exhibited rising R -curve behavior with toughening exponents of m = 0.042 and m = 0.135, respectively. AYP-SiC exhibited better flaw tolerance and more sharply rising R -curve behavior than AYE-SiC. The more sharply rising R -curve behavior and the better flaw tolerance of AYP-SiC were attributed mainly to grain bridging of crack faces by platelike grains. Because of the high degree of transgranular fracture, SS-SiC exhibited a flat R -curve despite a microstructural feature with platelike grains.     

R-Curve Behavior of Silicon Nitride–Titanium Nitride Composites

The R –curve for Si₃N₄−40 wt% TiN composites was estimated by the indentation-strength method and compared to that of monolithic Si3N4 with duplex microstructure. Both materials exhibited rising R -curve behavior. The Si3N4-TiN composites, however, displayed better damage tolerance and higher resistance to crack growth. From TEM observation, it was inferred that this superior performance of Si₃N₄-TiN composites can be attributed mainly to stress-induced microcracking at hete rophase (Si₃N₄/TiN) boundaries.     

Effect of Microcracking on the Thermal Diffusivity of Fe2TiO5

The effect of microcracking on the thermal diffusivity of polycrystalline Fe₂TiO₅ subjected to a range of annealing treatments was investigated. At fine grain size (∼1 μm), the thermal diffusivity exhibited the decrease with increasing temperature common for dielectrics. Extensive microcracking in the larger-grain-sized materials significantly decreased their thermal diffusivity. On heating, the microcracked materials exhibited increased thermal diffusivity at elevated temperatures which can be attributed primarily to microcrack closure and healing; on cooling, they exhibited a pronounced hysteresis, attributable to irreversible crack opening and closing. Thermal cycling closed the hysteresis curves, which suggests permanent changes in microcrack morphology. It appears that microcracking is a promising technique for tailoring ceramic materials to a combination of high thermal shock resistance and good insulating capability.     

R-Curve Behavior of Long Cracks in Alumina

Coarse-grained alumina is among those monolithic ceramics which can exhibit an increase in crack resistance with crack extension. This R -curve behavior is most pronounced for intergranular fracture and does not depend exclusively on material properties. Crack and specimen geometries also influence the shape of the R -curves. The magnitude of the effect increases with increasing crack surface roughness, which is microstructure-dependent, and with crack-opening displacement, which is geometry-dependent. Based on experimental observations, a "dynamic" R -curve model is presented which relates the increasing resistance to an increasing crack tip shielding caused by crack surface bridging. Applying a J -integral approach, R -curves are calculated for two specimen geometries (short double cantilever beam and single-edged notched beam) and different grain sizes. The good agreement between calculation and experiment indicates that the R -curve behavior of long cracks in alumina can be predicted by a simple wake model.     

Transformation Toughening in ZrO2-Containing Ceramics

Transformation toughening in ZrO₂-containing ceramics is discussed. Specifically, microstuctures of the three distinct types of ZrO₂-toughened ceramics are presented, after which microstructural evolution in MgO-partially-stabilized ZrO₂ Mg-PSZ) is reviewed. The mechanical properties of such transformation-toughened ceramics are dominated by "resistance-curve" ( R -curve) behavior, wherein the crack resistance increases during the course of crack propagation. Ceramics subject to R -curve behavior require a more detailed failure criterion than those subject to the usual linear elastic fracture mechanics criterion involving a critical stress intensity factor, K_IC.R -curve-controlled fracture in ceramics provides a degree of very desirable flaw insensitivity, but can lead to counterintuitive relationships concerning strength, toughness, and initial flaw size. Examples of R curves of Mg-PSZ with different thermal histories are given.     

Three-Dimensional Printing of Nanolaminated Ti3AlC2 Toughened TiAl3–Al2O3 Composites

Nanolaminates with a layered M _{N +1}AX _N crystal structure (with M: transition metal, A: group element, X: carbon or nitrogen, and N =1, 2, 3) offer great potential to toughen ceramic composites. A ternary Ti₃AlC₂ carbide containing ceramic composite was fabricated by three-dimensional printing of a TiC+TiO₂ powder mixture and dextrin as a binder. Subsequent pressureless infiltration of the porous ceramic preform with an Al melt at 800°–1400°C in an inert atmosphere, followed by reaction of Al with TiC and TiO₂ finally resulted in the formation of a dense multiphase composite of Ti₃AlC₂–TiAl₃–Al₂O₃. A controlled flaw/strength technique was utilized to determine fracture resistance as a function of crack extension. Rising R -curve behavior with increasing crack extension was observed, confirming the operation of wake-toughening effects on the crack growth resistance. Observations of crack/microstructure interactions revealed that extensive crack deflection along the (0001) lamellar sheets of Ti₃AlC₂ was the mechanism responsible for the rising R -curve behavior.     

Model for Toughness Curves in Two-Phase Ceramics: II, Microstructural Variables

The fracture mechanics analysis of Part I is here extended to consider the effects of volume fraction and scale of second-phase particles on the toughness-curve properties of ceramic-matrix composites. Increasing these variables enhances the flaw tolerance of the material, but only up to certain limits, beyond which bulk microcracking occurs. These limits define domains of damage accumulation and potential strength degradation by microcrack coalescence. In the familiar approximation of elliptical crack-wall profiles, we show that the principal effects of increasing volume fraction (or expansion mismatch) and particle size is to enhance the slope and scale of the T -curve, respectively. We also derive expressions for the microcracking limits and use these expressions to construct a simple design diagram for characterizing the effects of microstructural variation on mechanical behavior. Indentation-strength data on Al₂O₃ l Al₂TiO₅ composites over a range of volume fractions and particles sizes are used to demonstrate the severe loss in mechanical integrity that can be suffered on entering the microcracking domains.     

R-Curve Behavior and Thermal Shock Resistance of Ceramics

The influence of R -curve behavior of ceramics on the strength degradation associated with thermal shock is explored. Of particular significance for this interdependence is the observed nonlinear stress-strain behavior of materials that exhibit minimal strength degradation under severe thermal shock conditions. These two features, R -curve behavior and nonlinear behavior, are incorporated into a fracture mechanics analysis to provide a framework with which to understand severe thermal shock of ceramics. This analysis enables the estimation of the crack growth due to thermal shocking and also the anticipated strength degradation. The influence of specimen size is also addressed, and it is shown that greater strength degradation is anticipated with increasing specimen size. Experimental results for an alumina-zirconia composite material are presented to support the simple analysis.     

Thermal Shock Behavior of Duplex Ceramics

The thermal-stress fracture behavior of duplex ceramics is investigated by quenching in water and in oil. Comparison with the matrix materials shows that the critical quenching temperature difference, Δ T _c , is not or is only slightly reduced, even for duplex ceramics of significantly reduced strength. In sintered composites, thermal-stress-induced microcracking within pressure zones and crack initiation at pressure zone–matrix interfacial defects develop before Δ T _c is reached. The effects are accompanied by a gradual reduction in strength. At Δ T _c , critical crack propagation occurs. The retained strength after thermal shock of duplex ceramics is significantly improved compared with the respective matrix materials. This behavior can be related reasonably well with the K ^R -curve behavior.     

R-Curve Behavior of Si3N4–BN Composites

R -curve behavior of Si₃N₄–BN composites and monolithic Si₃N₄ for comparison was investigated. Si₃N₄–BN composites showed a slowly rising R -curve behavior in contrast with a steep R -curve of monolithic Si₃N₄. BN platelets in the composites seem to decrease the crack bridging effects of rod-shaped Si₃N₄ grains for small cracks, but enhanced the toughness for long cracks as they increased the crack bridging scale. Therefore, fracture toughness of the composites was relatively low for the small cracks, but it increased significantly to ∼8 MPa·m^1/2 when the crack grew longer than 700 μm, becoming even higher than that of the monolithic Si₃N₄.     

Influence of a Dispersion of Aluminum Titanate Particles of Controlled Size on the Thermal Shock Resistance of Alumina

The possibility of developing fine-grained (∼0.5–3 μm) and dense (≥0.98ρ_th) alumina (90 vol%)–aluminum titanate (10 vol%) composites with improved thermal shock resistance and maintained strength is investigated. One alumina material and one composite with similar microstructures (porosity and grain-size distribution) were fabricated to investigate the effect of Al₂TiO₅ on thermal shock behavior. The size of the Al₂TiO₅ particles was kept under 2.2 μm to avoid spontaneous microcracking. The mechanical and thermal properties of the materials involved in their response to thermal shock and the results for the evolution of indentation cracks of equal initial crack length with increasing Δ T in samples quenched in glycerine are described. The combination of thermal and mechanical properties—thermal conductivity, thermal expansion coefficient, Young's modulus, and toughness—improve the thermal shock resistance of the alumina–aluminum titanate composite in terms of critical temperature increment (>30%). The suitable structural properties of alumina—hardness and strength—are maintained.     

Effect of Temperature on Toughness Curves in Alumina

The effect of temperature on fracture strength and toughness curves ( T -curves) in the short-crack region of a polycrystalline alumina was studied. The indentation-strength technique was used to measure strength and T -curve behavior in the temperature range of 25° to 1300°C. Grain-localized crack bridging resulted in improved flaw tolerance and rising T -curves in this alumina. Both strength and toughness were observed to decrease with increasing temperature. A theoretical grain-bridging model was used to calculate the T -curves and fit to the experimental data. This allowed the evaluation of the temperature dependence of important bridging parameters.