R-Curve Behavior and Strength for In-Situ Reinforced Silicon Nitrides with Different Microstructures

R -curves for two in-situ reinforced silicon nitrides A and B of nominally the same composition are characterized using the Griffith equation and indentation fracture mechanics. These R -curves are calibrated against fine-grained silicon nitrides which have a known chevron-notch (long-crack) toughness and with a nearly flat R -curve behavior. Silicon nitride A, with its coarser microstructure and higher chevron-notch toughness, shows lower resitance to crack growth than silicon nitride B if the crack size is less than ∼200 μm. These results are consistent with the indentation–Strength measurements which show a crossover of strength between the two materials at an indentation load between 49 and 98 N, and below the crossover A has a lower strength. The toughening behavior is explained using an elastic-bridging model for the short crack, and a pullout model for the long crack. The effects of R -curve properties on design are discussed.     

R-Curve Behavior of Silicon Nitride Ceramic Reinforced with Silicon Carbide Platelets

Si₃N₄ ceramics reinforced with SiC platelets were fabricated by hot pressing at 1800°C. The microstructure of the Si₃N₄ matrix itself was the same with or without the addition of the SiC platelets. However, the mechanical properties of the Si₃N₄ were changed remarkably by the SiC addition. The fracture toughness and the crack resistance with crack propagation ( R -curve behavior) were improved while the fracture strength was decreased slightly by the platelets. Improvement in crack resistance was attributed to the extensive interaction of cracks with the platelets. The reduction in strength, on the other hand, is believed to be due to cracks associated with weak platelet-matrix interfaces.     

Crack-Healing Behavior of Liquid-Phase-Sintered Silicon Carbide Ceramics

Crack-healing behavior of liquid-phase-sintered (LPS) SiC ceramics has been studied as functions of heat-treatment temperature and crack size. Results showed that heat treatment in air could significantly increase the indentation strength. The heat-treatment temperature has a profound influence on the extent of crack healing and the degree of strength recovery. The optimum heat-treatment temperature depends on the softening temperature of an intergranular phase in each material. After heat treatment at the optimum temperature in air, the crack morphology almost entirely disappeared and the indentation strength recovered to the value of the smooth specimens at room temperature for the investigated crack sizes up to ∼200 μm. In addition, a simple heat treatment of SiC ceramics sintered with Al₂O₃–Y₂O₃–CaO at 1100°C for 1 h in air resulted in even further improvement of the strength, to a value of 1054 MPa (∼150% of the value of the unindented strength). Crack closure and rebonding of the crack wake due to oxidation of cracked surfaces were suggested as a dominant healing mechanism operating in LPS-SiC ceramics.     

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.     

High-Temperature Stiffness and Damping Measurements to Monitor the Glassy Intergranular Phase in Liquid-Phase-Sintered Silicon Carbides

Detailed stiffness and internal friction ( Q ⁻¹) versus temperature curves were obtained for liquid-phase-sintered silicon carbides using advanced resonant beam analysis up to 1400°C. As-sintered materials display a stable Q ⁻¹-peak near 1100°C, superimposed on an increasing background. The change of stiffness associated with the damping peak is quantitatively related to the amount of matter in pockets of the amorphous intergranular phase in which the refractory SiC matrix grains are embedded. The successful removal of the amorphous pockets by annealing at 1900°C is deduced from the disappearance of the damping peak and confirmed with transmission electron microscopy.     

Flaw-Tolerance and Crack-Resistance Properties of Alumina-Aluminum Titanate Composites with Tailored Microstructures

The microstructures of alumina-aluminum titanate (A-AT) composites have been tailored with the intent of altering their crack-resistance ( R - or T -curve) behavior and resulting flaw tolerance. Specifically, two microstructural parameters which influence grain-localized crack bridging, viz., (i) internal residual stresses and (ii) microstructural coarseness, have been investigated. Particulate aluminum titanate was added to alumina to induce intense internal residual stresses from extreme thermal expansion mismatch. It was found that A-AT composites with uniformly distributed 20–30 vol% aluminum titanate ("duplex") showed significantly improved flaw tolerance over single-phase alumina. Coarsening of the duplex microstructure via grain growth scaling was relatively ineffective in improving the flaw tolerance further. Onset of spontaneous microcracking precluded further exploitation of this scaling approach. Therefore, an alternative approach to coarsening was developed, in which a uniform distribution of large alumina grains was incorporated within a fine-grain A-AT matrix ("duplex-bimodal"), via a powder processing route. The duplex-bimodal composites yielded excellent flaw tolerance with steady-state toughness of ∼8 MPa˙m^1/2. A qualitative model for microstructure development in these duplex-bimodal composites is presented.     

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.     

Rising Crack-Growth-Resistance (R-Curve) Behavior of Toughened Alumina and Silicon Nitride

R -curves for a sinter/HIPed SiC(whisker)-reinforced alumina and a sintered silicon nitride were assessed by direct measurements of lengths of cracks associated with Vickers indentation flaws. The fracture toughness measurements based on (a) initial (as-indented) crack lengths, (b) equilibrium growth of cracks during increasing far-field loading, and (c) crack lengths corresponding to unstable fracture showed definitive trends of R -curves for both materials. The fracture mechanics analyses employed an indenter-material constant that was independently estimated using a physical model for the residual driving force and a free surface correction factor that accounted for the effects of size and shape of the cracks on stress intensity. It is shown that R -curve estimations based on crack length measurements have the intrinsic advantage that crack length dependence of fracture toughness is not assumed a priori as is done in conventional analysis based on strength. The measured fracture toughness of SiC(whisker)-reinforced alumina was in agreement with the prediction of a toughening model based on crack bridging by partially debonded whiskers.     

The AC Conductivity of Liquid-Phase-Sintered Silicon Carbide

Analysis of the AC conductivity, complex dielectric constant, and the resulting immittance spectra of liquid-phase-sintered silicon carbide (SiC) ceramics showed that for this system, the dominant experimental observations are due to a multicomponent grain-boundary phase and not due to SiC grains. This is confirmed by noting that the temperature dependence of the conductivity of the components, derived from the impedance spectra, is proportional to exp[−( T ₀/ T )^1/4] and not to exp[− C / T ]. The electrical properties of some of the grain boundaries are also found to be excitation voltage dependent. Combining the electrical results, which are also found to depend on the method of preparation and heat treatment, with a Rietveld analysis allows the composition of the grain boundaries of the models to be deduced.     

Effect of Weight Loss on Liquid-Phase-Sintered Silicon Carbide

The evaporation of silicon carbide (SiC) ceramics during sintering has been studied by thermogravimetry in a graphite furnace filled with argon. The SiC powder compacts contained 7.5 wt% eutectic composition of Y₂O₃–Al₂O₃ to promote liquid-phase sintering. A weight loss of 1–11 wt% was observed during sintering, depending on the sintering temperature and sintering time. The weight loss severely influenced the final density and the microstructure of the SiC ceramics. Particularly, the oxide sintering aids, which were homogeneously distributed in the green ceramics, were observed to segregate and form particular patterns that were dependent on the temperature, sintering time, and the total weight loss. Possible heterogeneous reactions evolving volatile species have been discussed in relation to the experimental observations.     

Measurement of Rising R-Curve Behavior in Toughened Silicon Nitride by Stable Crack Propagation in Bending

A simple procedure for measuring the R -curve properties of ceramics by a stable fracture test in three-point bending is described. As a typical case, data are displayed for a Si₃N₄ material toughened by the presence of acicular grains in situ grown during the sintering process. The fracture mechanics specimen was a single-edge double-notched beam (SEDNB), whose notch was sharpened to a radius of <10 μm in order to reduce the amount of elastic energy stored at its root prior to crack extension. Furthermore, a stabilizer, specially designed for the bending geometry, was used to control crack stability. During stable extension, the crack could be easily arrested at selected locations of the load-displacement curve, the load quickly released, and the stable crack extension directly measured by the die-penetration technique. The crack resistance, K _R, of the material was calculated from the measured crack extent and the onset load value before unloading. This method enabled us to precisely monitor the critical load value at which the load-displacement curve deviated from linear behavior, as well as crack extensions from a few tens of micrometers to about 1 mm. As an application of this method, the fracture resistance of a Si₃N₄ material with rising R -curve behavior was measured and found to increase from about 5.5 to 9.0 MPaμm^1/2 within a 0.8-mm extension.     

Core/Rim Structure of Liquid-Phase-Sintered Silicon Carbide

Plasma etching in conjunction with scanning and analytical transmission electron microscopy was used to characterize the microstructure and microchemistry of silicon carbide sintered with yttrium-aluminum garnet (YAG). The SiC grains comprise a core/rim structure with small amounts of excess yttrium, aluminum, and oxygen being present in the rim while these elements are missing in the core. The core/rim interface was found to be coherent, and both the core and the rim are composed of the same polytype, predominantly the 6H structure. These results suggest that Ostwald ripening by solution and reprecipitation controls the sintering mechanism in this system.     

Long Crack R-Curve of Aligned Porous Silicon Nitride

Long crack R -curve of a porous Si₃N₄ with aligned fibrous grains was investigated, using a chevron-notched beam technique. A crack was constrained to propagate normal to the grain alignment. The crack growth resistance of aligned porous Si₃N₄ was much larger compared with that of dense Si₃N₄ ceramics. Microstructure observations showed that pullouts of fibrous grains in aligned porous Si₃N₄ markedly increased during crack propagation relative to those of dense Si₃N₄, due to the existence of pores. The efficient grain pullouts in porous Si₃N₄ increased the bridging stress at the crack wake.     

Elevated-Temperature R-Curve Behavior of a Polycrystalline Alumina

The fracture behavior of a polycrystalline alumina was examined at temperatures ranging from ambient through 1400°C, using three-point bend bar test specimens. R -curves were determined at all temperatures studied, and when accompanied by renotching procedures, a wake removal technique, conclusive evidence was provided to support the existence of a following wake region in this monolithic ceramic material. The crack closure stresses identified in this region are responsible for all toughening with crack extension observed in this study. Room-temperature " K _IC" fracture toughness values of 4.5 MPa · m^1/2 for the chevron-notch specimen and 3.9 MPa · m^1/2 for the straight-notch configuration were obtained. The critical stress intensity factor of the renotched chevron-notch specimen compared very closely with that of the straight-notch specimen. These findings further confirm the toughening role of the microstructural features found in the following wake region. This paper considers, in detail, these observations in terms of the microstructure and its role in the toughening mechanism.     

Subcritical Crack Growth of Macrocracks in Alumina with R-Curve Behavior

Subcritical crack growth of macroscopic cracks in two Al₂O₃ ceramics is investigated with single-edge-notched bending specimens under constant load. The resulting v - K _I-curves are in complete contrast to the behavior of natural cracks. In spite of the monotonic increase of the externally applied stress intensity factor due to crack extension, the crack growth rates first decrease. This behavior is caused by crack shielding due to crack border interaction and can be described by a rising crack growth resistance. Two methods are applied to determine the R -curve under subcritical crack growth conditions.     

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.     

工程陶瓷材料的阻力曲线行为

本文简要说明了工程陶瓷材料裂纹扩展阻力曲线（Ｒ－Ｃｕｒｖｅ）行为的理论基础，阐述了陶瓷材料阻力曲线行为研究的历史和现状，并对目前研究中存在的问题做了评述，提出了进一步探讨的方向。     

Grain-Boundary Viscosity of Polycrystalline Silicon Carbides

Internal friction experiments were conducted on three SiC polycrystalline materials with different microstructural characteristics. Characterizations of grain-boundary structures were performed by high-resolution electron microscopy (HREM). Observations revealed a common glass-film structure at grain boundaries of two SiC materials, which contained different amounts of SiO₂ glass. Additional segregation of residual graphite and SiO₂ glass was found at triple pockets, whose size was strongly dependent on the amount of SiO₂ in the material. The grain boundaries of a third material, processed with B and C addition, were typically directly bonded without any residual glass phase. Internal friction data of the three SiC materials were collected up to similar/congruent2200°C. The damping curves as a function of temperature of the SiO₂-bonded materials revealed the presence of a relaxation peak, arising from grain-boundary sliding, superimposed on an exponential-like background. In the directly bonded SiC material, only the exponential background could be detected. The absence of a relaxation peak was related to the glass-free grain-boundary structure of this polycrystal, which inhibited sliding. Frequency-shift analysis of the internal friction peak in the SiO₂-containing materials enabled the determination of the intergranular film viscosity as a function of temperature.     

Creep and Microstructural Evolution at High Temperature of Liquid-Phase-Sintered Silicon Carbide

The compressive creep characteristics at 1625°C of liquid-phase-sintered silicon carbide ceramics containing 5 and 15 wt% of crystalline Y₃Al₅O₁₂ (YAG) as the secondary phase were studied. In the two cases, strains between 10% and 15% were reached without failure. The creep behavior was characterized by a stress exponent n ≈2, and the proportion of secondary phase was related to the creep resistance of the materials. The microstructural evolution during creep consisted firstly in the re-distribution of the secondary phase, probably as a consequence of its viscous flow at the creep conditions, and secondly an extensive nucleation and growth of cavities, which was more important for the highest YAG content. The latter reflects the carbothermal reduction that the secondary phase undergoes during creep.     

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.