Mixed-Mode Fracture from Controlled Surface Flaws in Hot-Pressed Si3N4

The room-temperature mixed-mode fracture of commercial hot-pressed Si₃N₄ was examined using controlled surface flaws in 4-point bending, oriented at various angles 6 with respect to the outer fiber tensile stress direction. Catastrophic fracture paths were non-coplanar with the initial flaw plane, and the stress intensity factor ratio K_I/K_IC was < 1 for fracture in modes II and III. A non-coplanar maximum strain-energy release rate fracture criterion best described mixed-mode fracture.     

Crack Healing and Stress Relaxation in Al2O3 SiC "Nanocomposites"

The crack-healing behavior of A1₂O₃ and Al₂O₃-SiC nanocomposite was studied using Vickers indentations to generate precracks. After annealing in argon for 2 h at 1300°C, radial cracks in the nanocomposite healed: The cracks closed and there was a small degree of rebonding in the vicinity of the crack tip. In contrast, radial cracks in alumina grew when exposed to the same annealing treatment. The different responses are attributed to the fracture mode and toughening mechanism in each material: In the nanocomposite, the cracks close as the residual stresses surrounding the indentations relax. Radial cracks open and grow in A1₂O₃ because microstructural toughening is diminished during heating to the annealing temperature. An implication is that strength-limiting machining flaws in these materials behave similarly, thereby accounting for the strengthening effect of annealing in this "nanocomposite" system.     

Comparison of KIc Values for Al2O3-ZrO2 Composites Obtained from Notched-Beam and Indentation Strength Techniques

Values of K_Icfor hot-pressed AL₂O₃-ZrO₂ composites were measured using notched-beam and indentation strength techniques. The results are compared with K factors at the mirror/mist boundary and at crack branching. It was found that the indentation strength technique provides a more consistent estimation of K_Ic, than the notched-beam technique.     

Controlled Surface Flaws in Hot-Pressed Si3N4

Surface flaws of controlled size and shape were produced in high-strength hot-pressed Si₃N₄ with a Knoop microhardness indenter. Fracture was initiated at a single suitably oriented flaw on the tensile surface of a 4-point-bend specimen, with attendant reduction in the measured magnitude and scatter of the fracture strength. The stress required to propagate the controlled flaw was used to calculate the critical stress-intensity factor, K _IC, from standard fracture-mechanics formulas for semielliptical surface flaws in bending. After the bend specimen had been annealed, the room-temperature K _IC values for HS-130 Si₃N₄ increased to a level consistent with values obtained from conventional fracture-mechanics tests. It was postulated that annealing reduces the residual stresses produced by the microhardness indentation. The presence of residual stresses may account for the low K _IC, values. Elevated-temperature K_IC values for HS-130 Si₃N₄ were consistent with double-torsion data. Controlled flaws in HS-130 Si₃N₄ exhibited slow crack growth at high temperatures.     

R Curves and Crack-Stability Map: Application to Ce-TZP/Al2O3

The concept of a crack-stability map is developed by considering the interaction between the crack-driving force and the rising crack-growth resistance of a toughened ceramic. The map plots normalized transition crack length as function of the ratio of the crack-initiation fracture toughness and the plateau toughness to delineate regimes of stable and unstable crack growth. The plot is used to analyze R curves and fracture stresses of a transformation-toughened Ce-TZP/Al₂O₃. It is shown that the fracture stress and the small scatter measured for this ceramic are consistent with its R- curve behavior, which enables stable growth of surface cracks from flaws (pores and second-phase particles), leading to a flaw-insensitive ceramic.     

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.     

Relationship Between Microstructures and Material Properties of Novel Fibrous Al2O3–(m-ZrO2)/t-ZrO2 Composites

Novel fibrous Al₂O₃–(m-ZrO₂)/t-ZrO₂ (m, monoclinic; t, tetragonal) composites having a core/shell structure were fabricated by multi-extrusion, and their microstructures and material properties were investigated depending on the number of extrusions. The composites acquired a homogeneously fine fibrous structure as the number of extrusions increased. The bending strength and fracture toughness increased remarkably as the number of extrusions increased. In the fracture surface of the second passed composite, an Al₂O₃–(m-ZrO₂) core region appeared, flat type, although some local regions existed with an intergranular fracture. However, the fracture mode of the t-ZrO₂ region was of intergranular type having a sharp and rough surface. In the composite made by the fifth passed extrusion, the fracture strength and toughness values were high at about 665 MPa and 9.6 MPa·m^1/2, respectively. The main fracture mode was a typical intergranular mode having a rough fracture surface, and the main multi-toughening was because of mechanisms such as crack bridging, microcracking, and phase transformation.     

Slow Crack Growth from Controlled Surface Flaws in Hot-Pressed Si3N4

The elevated-temperature slow-crack-growth behavior of HS-130 Si₃N₄ was studied by extending "controlled" surface cracks in bars loaded in 4-point bending. Several such nonin-teracting cracks were produced on the tensile surfaces of bend bars by Knoop microhardness indentation. The stress and dimensions of the subcritically growing cracks were used to calculate the stress-intensity factor, K₁ , from fracture-mechanics formulas for semielliptical surface cracks in bending. The crack-growth velocity, v, was obtained by dividing crack extension by loading time interval. The data indicated very large scatter in measured velocities for given K₁ values, which was interpreted as due to the interaction of the small cracks with local material heterogeneities. No simple functional relation between K _I and v could be established for HS-130 Si₃N ₄ from the v − K ₁ data.     

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.     

KIc and Delayed Fracture Measurements on Hot-Pressed SiC

The fracture resistance of hot-pressed SiC between 300 and 1773 K was measured using K_Ic , and notched-beam delayed-fracture tests. An analysis was developed which enables crack velocities as low as 10⁻¹¹ ms⁻¹ to be derived from the failure time.     

Slow Crack Growth Behavior in Transformation-Toughened Al2O3-ZrO2(Y2O3) Ceramics

Significant increases in the critical fracture toughness (K _IC ) over that of alumina are obtained by the stress-induced phase transformation in partially stabilized ZrO₂ particles which are dispersed in alumina. More importantly, improved slow crack growth resistance is observed in the alumina ceramics containing partially stabilized ZrO₂ particles when the stress-induced phase transformation occurs. Thus, increasing the contribution of the ZrO₂ phase transformation by tailoring the Y₂O₃ stabilizer content not only increases the critical fracture toughness (K_IC) but also the K _Ia to initiate slow crack growth. For example, crack velocities ( v )≥10^–9 m/s are obtained only at K _Ia≥5 MPa.m^1/2 in transformation-toughened ( K _IC=8.5 MPa.m^1/2) composites vs K _Ia≥2.7 MPa.m^1/2 for comparable velocities in composites where the transformation does not occur ( K _IC=4.5 MPa.m^1/2). This behavior is a result of crack-tip shielding by the dissipation of strain energy in the transformation zone surrounding the crack. The stress corrosion parameter n is lower and A greater in these fine-grained composite materials than in fine-grained aluminas. This is a result of the residual tensile stresses associated with larger (≥1 μm) monoclinic ZrO₂ particles which reside along the intergranular crack path.     

Fractographic Criteria for Subcritical Crack Growth Boundaries in 96% Al2O3

The percent intergranular fracture (PIF) was measured along radii extending from fracture origins in 96% A1₂O₃ specimens, fractured at various loading rates and temperatures, and plotted vs estimates of stress intensity factors ( K ₁) at the corresponding crack lengths. Two types of curves were observed. The first was similar to curves previously observed for hot-pressed alumina. In this case the subcritical crack-growth boundary was located approximately where the minimum in the PIF occurred near K ₁=4MPa·m^½, as was also the case for hotpressed alumina. Therefore, the location of this minimum or the projecting grams formed by intergranular fracture as the crack velocity increased can be used as criteria for locating the subcritical crack-growth boundary. The second type of curve lacks the minima in PIF characteristic of the first type and is characterized by a gradual trend toward higher PIF beginning at K ₁=3MPa·m^½. This type of curve may be caused by acceleration of the crack to high crack velocities at values of K ₁ approximately equal to or slightly greater than those necessary to cause critical crack growth on the lower fracture-energy planes in sapphire. Assuming that this is the case, the K ₁ at which the trend toward higher PIF begins can be used to calculate the radius to the critical flaw boundary for this type of fracture.     

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.     

Factor Analysis of Fracture-Toughness Test Parameters for Al2O3

The double-cantilever-beam technique was used to determine the effects of varying 6 factors related to specimen preparation, size, and testing conditions on the fracture toughness of polycrystalline Al₂O₃. Experimental design and statistical factor analysis techniques were used to investigate each factor at two levels. Direct fracture surface replication and electron microscopy provided supporting information about the fracture mode and fracture surface features for each test condition. The fracture toughness of Al₂O₃ was higher for 30-μm grain size than for 10-μm grain size. Pretest annealing (900°C) and specimen width were both significant factors for 10-μm Al₂O₃. The effects of variations of beam width, beam height, and test machine speed were masked by data scatter and are being studied further. The ratio of specimen width to fracture web width caused no effect in the range studied. The sensitivity of the test results to sample dimensions and surface finish is small enough that special care in cutting and measuring of samples is not required.     

Fracture Toughness and Spalling Behavior of High-Al2O3 Refractories

The fracture energies and spalling resistance of high-Al₂O₃ refractories were studied. The fracture energies, γ _WOF and γ _NBT , were measured by the work-of-fracture and the notched-beam-test methods, respectively. Spalling resistance, as measured by the relative strength retained in a water quench, correlated well with the thermal-stress resistance parameter applicable to stable crack propagation under conditions of thermal shock, (γ _WOF /α² E ₀). Many of the refractories exhibited high ratios of γ_WOF to γ_NBT; such high ratios were shown analytically to maximize the parameter ( R ¹¹¹¹= E _0γWOF/S₁²) which describes the resistance to catastrophic spalling. The increase of crack length with increasing quenching temperature difference (Δ T ) was somewhat less than that predicted theoretically; the discrepancy was attributed to an increase of crack density with Δ T . In general, the results show that fracture energy is important in establishing the spalling resistance of high-Al₂O₃ refractories.     

Influence of Cu2O and CuAlO2 Interphases on Crack Propagation at Cu/α-Al2O3 Interfaces

In-situ crack-propagation experiments, in conjunction with thermochemical experiments, have been used to examine the role of discontinuous interphases on the fracture behavior of solid-state diffusion-bonded Cu/α-Al₂O₃ couples. Clean, interphase-free interfaces exhibit crack extension by brittle decohesion at the crack tip at an initiation fracture energy of 125 J/m². Crack propagation is characterized by an increase in the fracture energy with increases in the crack length ( R -curve behavior). When interfacial chemical reaction products are present, the crack growth is altered, depending on the characteristics of the interphase. The presence of Cu₂O needles results in preferential debonding along the Cu₂O/Al₂O₃ interface. On the other hand, finer CuAlo₂ needles visibly impede crack propagation and result in a higher interface initiation fracture energy (}190 J/m²) than that of the interphase-free interface. The effects of the Cu₂O and CuAlo₂ phases on the fracture energy are discussed.     

Indentation Studies on Y2O3-Stabilized ZrO2: II, Toughness Determination from Stable Growth of Indentation-Induced Cracks

Stable indentation cracks were grown in four-point bend tests to study the fracture toughness of two Y₂O₃-stabilized ZrO₂ ceramics containing 3 and 4 mol% Y₂O₃. By combining microscopic in situ stable crack growth observations at discrete stresses with crack profile measurements, the dependence of toughness on crack extension was determined from crack extension plots, which graphically separate the crack driving residual stress intensity and applied stress intensity factors. Both materials exhibit steeply rising R -curves, with a plateau toughness of 4.5 and 3.1 Mpa·m^1/2 for the 3- and 4-mol% materials, respectively. The magnitude of the plateau toughness reflects the fraction of tetragonal grains contributing to transformation toughening.     

Enhanced Fracture Toughness in Layered Microcomposites of Ce-ZrO2 and Al2O3

Laminar composites, containing layers of Ce-ZrO₂ and either Al₂O₃ or a mixture of Al₂O₃ and Ce-ZrO₂, have been fabricated using a colloidal method that allowed formation of layers with thicknesses as small as 10 μm. Strong interactions between these layers and the martensitic transformation zones surrounding cracks and indentations have been observed. In both cases, the transformation zones spread along the region adjacent to the layer, resulting in an increased fracture toughness. The enhanced fracture toughness was observed for cracks growing parallel to the layers as well as for those that were oriented normal to the layers.     

Strength-Toughness Relations in Sintered and Isostatically Hot-Pressed ZrO2-Toughened Al2O3

The fracture toughness of fine-grained undoped ZrO₂-toughened Al₂O₃ (ZTA) was essentially unchanged by postsintering hot isostatic pressing and increased monotonically with ZrO₂ additions up to 25 wt%. The strength of ZTA with 5 to 15 wt% tetragonal ZrO₂, which depended monotonically on the amount of ZrO₂ present before hot isostatic pressing, was increased by pressing but became almost constant between 5 and 15 wt% ZrO₂ addition. The strength appeared to be controlled by pores before pressing and by surface flaws after pressing; the size of flaws after pressing increased with ZrO₂ content. The strength of ZTA containing mostly monoclinic ZrO₂ (20 to 25 wt%) remained almost constant despite the noticeable density increase upon hot isostatic pressing because the strength was controlled by preexisting microcracks whose extent did not change on postsintering pressing. These strength-toughness relations in sintered and isostatically hot-pressed ZTA are explained on the basis of R -curve behavior. The importance of the contribution of microcracks to the toughness of ZTA is emphasized.     

Reinforcement of Hydroxyapatite Bioceramic by Addition of Ni3Al and Al2O3

The effects of Ni₃Al and Al₂O₃ additions on the mechanical properties of hydroxyapatite (HAp) were investigated. The addition of Ni₃Al particles increased the strength as well as the fracture toughness of HAp. However, the improvements in the properties were limited because of the formation of microcracks around the metal particles. The microcracks were formed because of the large difference in the coefficients of thermal expansion between HAp and Ni₃Al, and because of the relatively large size of Ni₃Al particles (∼20 µm). The addition of submicrometer Al₂O₃ powder was also effective in increasing the mechanical properties. The flexural strength and the fracture toughness were increased from about 100 MPa and 0.7 MPam^1/2, respectively, to 200 MPa and 1.5 MPam^1/2 by the addition of 20 vol% Al₂O₃. When Ni₃Al and Al₂O₃ were added together, the fracture toughness was further increased to 2.3 MPam^1/2. This increase in the fracture toughness was attributed to the synergistic effect of matrix strengthening and crack interactions with the metal particles.