Tensile Creep Behavior of Alumina/Silicon Carbide Nanocomposite

Tensile creep and creep rupture behaviors of alumina/17 vol% silicon carbide nanocomposite and monolithic alumina Were investigated at 1200° to 1300°C and at 50 to 150 MPa. Compared to the monolithic alumina, the nanocomposite exhibited excellent creep resistance. The minimum creep rate of the nanocomposite was about three orders of magnitude lower and the creep life was 10 times longer than those of the monolith. The nanocomposite demonstrated transient creep until failure, while accelerated creep was observed in the monolith. It was revealed that rotating and plunging of intergranular silicon carbide nanoparticles into the alumina matrix increased the creep resistance with grain boundary sliding.     

Reaction sintering of alumina/mullite nanocomposites from nano-sized starting powders

Alumina/mullite ceramic nanocomposites were prepared by the mixtures of nano-sized starting powders of alumina with silica and alumina with silicon carbide. Silica from deliberate addition and as the product of silicon carbide oxidation reacted completely with alumina to form mullite. Silica from direct addition segregated at the grain boundary and intergranular mullite was formed whereas silica from oxidation was surrounded by alumina matrix and intragranular mullite was formed after reaction sintering. The most significant difference was fracture behaviour where intragranular mullite nanoparticles promoted transgranular fracture in alumina matrix due to thermal mismatch around nanoparticles and intergranular mullite nanoparticles gave rise to intergranular fracture similar to pure alumina. Wear resistance of the nanocomposites was better than that of alumina. Pull-out formation in the nanocomposites was less and pull-out size was also smaller. Fracture toughness of the nanocomposites was significantly higher than that of alumina.     

On the Effect of Local Grain-Boundary Chemistry on the Macroscopic Mechanical Properties of a High-Purity Y2O3-Al2O3-Containing Silicon Nitride Ceramic: Role of Oxygen

The effects of grain-boundary chemistry on the mechanical properties of high-purity silicon nitride ceramics have been investigated, specifically involving the role of oxygen, present along the grain boundaries, in influencing the fracture behavior. To avoid complications from inadvertently introduced impurities, studies were performed on a high-purity Si₃N₄ processed using two-step gas-pressure-HIP sintering. Varying the grain-boundary oxygen content, which was achieved by control of oxidizing heat treatments and sintering additives, was found to result in a transition in fracture mechanism, from transgranular to intergranular fracture, with an associated increase in fracture toughness. This phenomenon is correlated to an oxygen-induced change in grain-boundary chemistry and possibly to a concomitant structural transformation along the interface. The incorporation of oxygen appears to affect fracture by "weakening" the interface, thus facilitating debonding and crack advance along the boundaries, and hence to toughening by grain bridging. It is concluded that if the oxygen content in the thin grain-boundary films exceeds a lower limit, which is ∼0.87 equiv% oxygen content, then the interfacial structure and bonding characteristics favor intergranular debonding during crack propagation; otherwise, transgranular fracture ensues.     

Solid-Sample 11B Nuclear Magnetic Resonance and X-ray Photoelectron Spectroscopy Study of Boron-Doped β-Silicon Carbide

Solid-sample magic angle spinning (MAS) nuclear magnetic resonance (NMR) and X-ray photoelectron spectroscopy (XPS), in conjunction with scanning electron microscopy (SEM), were used to investigate the fate of boron used as a sintering aid for silicon carbide. The results of the NMR studies indicated that the boron penetrated the silicon carbide grain boundaries during sintering, and was incorporated in a tetrahedral form in the bulk, regardless of the gas used during the process. The NMR spectrum of a sample sintered under nitrogen indicated the formation of a trigonal form of boron as well. XPS identified this trigonal boron as boron nitride; however, no boron was detected by XPS in any form on the fracture surface of the silicon carbide sintered under argon, even though the NMR results confirmed the presence of tetrahedral boron in the bulk sample. The SEM results indicated that the fracture process for these materials was predominantly intergranular. This suggested that the boron in the silicon carbide sintered under argon penetrated the grains and left the grain boundaries depleted of boron.     

Effect of Microstructure on the Creep of Siliconized Silicon Carbide

Mechanisms of creep deformation have been investigated for a commercial grade of siliconized carbide containing ≅33%/silicon. Microstructural studies of both tensile and compressive test specimens indicate dislocation damage generation in both the silicon carbide and the silicon phases as a consequence of creep. In the silicon carbide, dislocation damage was normally restricted to contact sites between the silicon carbide grains resulting from high intergranular contact stresses during deformation. Dislocation damage was also observed in the silicon. Although dislocation damage was heavy in some regions of the specimens, most regions of the specimens, most regions were free of dislocations. This result is consistent with the hypothesis that deformations occurs by the motion of clusters of grains during deformation. In tension, creep at high strain rates, 1 × 10⁻⁸_S⁻¹, was accompanied by the formation of cavities at Si/SiC interfaces within the intergranular silicon phase. As cavities were not associated with dislocations, their growth was probably controlled by diffusional processes. Based on observations of the microstructure, a model of deformation is proposed to explain the fact that siliconized silicon carbide creeps faster in tension than in compression, at the same applied stress. The model is based on soil mechanics concepts. It is suggested that creep is controlled by intergranular friction between aggregate particles of the composite.     

Diffusional Crack Growth and Creep Rupture of Silicon Carbide Doped with Alumina

This study deals with tensile creep and crack growth behavior of silicon carbide doped with alumina at 1400°C. Excellent creep resistance was observed for stresses from 150 MPa to 200 MPa. From the creep exponent of 1.4 and the activation energy of 320 kj/mol, the principal creep mechanism was Coble creep. The creep failure was caused by slow crack growth from a preexisting flaw. The crack was found to grow subcritically along grain boundaries almost in isolation. The relation between the time–to–failure and the applied stress was well treated by a diffusive crack growth model, and the threshold stress of this material at 1400°C was estimated at 165 MPa.     

Grain boundary glasses in silicon nitride: A review of chemistry,properties and crystallisation

Silicon nitride for engineering applications is densified by liquid phase sintering using oxide additives such as yttria and alumina. The oxynitride liquid remains as an intergranular glass. This paper provides a review of microstructural development in silicon nitride, grain boundary oxynitride glasses and effects of chemistry on properties. Nitrogen increases T_g, viscosities, elastic moduli and microhardness. These property changes are compared with known effects of grain boundary glass chemistry in silicon nitride ceramics where significant improvements in fracture resistance of silicon nitride can be achieved by tailoring the intergranular glass chemistry.Crystallisation of the grain boundary Y–Si–Al–O–N glass phase can improve properties. Nucleation and crystallisation of a Y–Si–Al–O–N glass, similar to that found in grain boundaries of silicon nitride densified with yttria and alumina, can be optimised to form different Y-disilicate polymorphs at different temperatures. One solution to provide a single disilicate phase over a range of temperatures is discussed.     

Effect of Microstructure on Material-Removal Mechanisms and Damage Tolerance in Abrasive Machining of Silicon Carbide

Effects of microstructural heterogeneity on material-removal mechanisms and damage-formation processes in the abrasive machining of silicon carbide are investigated. It is shown that the process of material removal in a conventional silicon carbide material with equiaxed-grain micro-structure and strong grain boundaries consists of the formation and propagation of transgranular cracks which results in macroscopic chipping. However, in a silicon carbide material, containing 20 vol% yttrium aluminum garnet (YAG) second phase, with elongated-grain micro-structure and weak grain boundaries, intergranular micro-cracks are formed at the interphase boundaries, leading to dislodgment of individual grains. These different mechanisms of material-removal affect the nature of machining-induced damage. While in the conventional silicon carbide material the machining damage consists of transgranular median/radial cracks, in the heterogeneous silicon carbide material, abrasive machining produces interfacial micro-cracks distributed within a thin surface layer. These two distinct types of machining damage result in a different strength response in the two forms of silicon carbide materials. In the case of the conventional silicon carbide, grinding damage results in a dramatic decrease in strength relative to the as-polished specimens. In contrast, the ground heterogeneous silicon carbide specimens show no strength loss at all.     

Processing and fracture behaviour of hot pressed silicon carbide whisker reinforced alumina

The improvement of mechanical properties of silicon carbide whisker reinforced alumina has been investigated with emphasis on the effects of the whisker type and content, the hot pressing temperature and the influence of an interfacial film between the whisker and the matrix. The introduction of silicon carbide whiskers significantly improves the fracture toughness, flexural strength and creep resistance of polycrystalline alumina.

However, these properties are strongly dependent on the size and morphology of whiskers. Large diameter whiskers generate extensive micro-cracking which leads to a decrease in flexural strength. Also, the presence of carbon-coated SiC whiskers substantially increases the high temperature strain rate by promoting cavitation. A grain boundary glassy phase introduced by the carbon coating was also detected.     

Voronoi cell finite element modelling of the intergranular fracture mechanism in polycrystalline alumina

The mechanisms of fracture in polycrystalline alumina were investigated at the grain level using both the micromechanical tests and finite element (FE) model. First, the bending experiments were performed on the alumina microcantilever beams with a controlled displacement rate of 10 nm s^–1 at the free end; it was observed that the intergranular fracture dominates the failure process. The full scale 3D Voronoi cell FE model of the microcantilever bending tests was then developed and experimentally validated to provide the insight into the cracking mechanisms in the intergranular fracture. It was found that the crystalline morphology and orientation of grains have a significant impact on the localised stress in polycrystalline alumina. The interaction of adjacent grains as well as their different orientations determines the localised tensile and shear stress state in grain boundaries. In the intergranular fracture process, the crack formation and propagation are predominantly governed by tensile opening (mode I) and shear sliding (mode II) along grain boundaries. Additionally, the parametric FE predictions reveal that the bulk failure load of the alumina microcantilever increases with the cohesive strength and total fracture energy of grain boundaries.     

Silicon nitride–silicon carbide micro/nanocomposites: A review

This paper reviews investigations of silicon nitride–silicon carbide micro–nanocomposites from the original work of Niihara, who proposed the concept of structural ceramic nanocomposites, to more recent work on strength and creep resistance of these unique materials. Various different raw materials are described that lead to the formation of nanosized SiC within the Si₃N₄ grains (intragranular) and at grain boundaries (intergranular). The latter exert a pinning effect on the amorphous grain boundary phases in the silicon nitride and also act as nucleation sites for β-Si₃N₄, which limits grain growth during sintering. This finer microstructure results in strengths higher than for the monolithic silicon nitride. Intragranular SiC particles enhance strength and fracture toughness as a result of residual compressive thermal stresses within the nanocomposites. High temperature strength and creep resistance are also much higher than for monolithic silicon nitride and a few investigations of these topics are briefly reviewed and the proposed mechanisms are described. Within the context of other studies cited, work on Si₃N₄–SiC micro–nanocomposites by the current authors describes an aqueous processing route for better dispersion of commercial powders prior to sintering.     

Structural design and energy absorption mechanism of laminated SiC/BN ceramics

The laminated silicon carbide/boron nitride (SiC/BN) ceramics with different structural designs were fabricated by pressureless sintering at 1900?°C for 1?h in argon flow. The alumina (Al₂O₃)-and yttrium(III) oxide (Y₂O₃)-doped SiC ceramic exhibited a significant intergranular fracture behavior, which could be attributed to the yttrium aluminum garnet (YAG) phase located at the grains boundaries. The bending strength and fracture toughness were used to characterize the crack propagation including the delamination cracking, crack kinking, and crack deflection. The energy absorption in the process of crack propagation was characterized by the work of fracture (WOF) and damping capacity. The mode of crack propagation changed with the change in the structure and variation of BN content in the BN layer. The delamination cracks occurred inside the BN layer or at the interface between SiC and BN layers. The sample with a gradient structure exhibited the combination of delamination cracks occurring at the interface and inside the BN layer, which showed the maximum WOF of 2.43?KJ?m^?2, bending strength of 300?MPa, and fracture toughness of 8.5?MPa?m^1/2. The damping capacity varied with the change of the structure and the amplitude. The sample with a gradient structure exhibited the damping capacity of 0.088 and the maximum loss modulus of 9.758?GPa.     

Fracture and Fatigue Behavior at Ambient and Elevated Temperatures of Alumina Bonded with Copper/Niobium/Copper Interlayers

Interfacial fracture toughness and cyclic fatigue-crack growth properties of joints made from 99.5% pure alumina partially transient liquid-phase bonded using copper/niobium/copper interlayers have been investigated at both room and elevated temperatures, and assessed in terms of interfacial chemistry and microstructure. The mean interfacial fracture toughness, G _c, was found to decrease from 39 to 21 J/m² as temperature was raised from 25° to 1000°C, with failure primarily at the alumina/niobium interfaces. At room temperature, cyclic fatigue-crack propagation occurred both at the niobium/alumina interface and in the alumina adjacent to the interface, with the fatigue threshold, Δ G _TH, ranging from 20 to 30 J/m²; the higher threshold values in that range resulted from a predominantly near-interfacial (alumina) crack path. During both fracture and fatigue failure, residual copper at the interface deformed and remained adhered to both sides of the fracture surface, acting as a ductile second phase, while separation of the niobium/alumina interface appeared relatively brittle in both cases. The observed fracture and fatigue behavior is considered in terms of the respective roles of the presence of ductile copper regions at the interface which provide toughening, extrinsic toughening due to grain bridging during crack propagation in the alumina, and the relative crack propagation resistance of each crack path, including the effects of segregation at the interfaces found by Auger spectroscopy.     

Thickness Alteration of Grain-Boundary Amorphous Films during Creep of a Multiphase Silicon Nitride Ceramic

Experimental observations of the creep response of a commercial sintered silicon nitride ceramic are presented. The stable microstructure of this material at high temperature contains secondary crystalline phases which result from partial devitrification of the intergranular phase. The widths of amorphous films along grain boundaries (between silicon nitride grains) and phase boundaries (between silicon nitride and secondary phase grains) are characterized by transmission electron microscopy. The thickness distributions of grain-boundary films before and after creep are analyzed by a statistical method. While the film widths are highly uniform before creep, a bimodal distribution is observed after creep. The results suggest that viscous flow of the boundary amorphous films occurs during creep deformation.     

Microstructure and mechanical properties of alumina ceramics reinforced by boron nitride nanotubes

Boron nitride nanotubes (BNNTs)/alumina composites were fabricated by hot pressing. The mechanical properties of the composites are greatly dependent upon the content of BNNTs. In comparison with monolithic alumina, the incorporation of BNNTs results in the improvement of bending strength and fracture toughness owing to the effective inhibition of grain growth. A routine toughening mechanism, especially the bridging of BNNTs at grain boundaries and the sufficient physical bonding between BNNTs and alumina matrix, is dominantly responsible for the increase in mechanical properties.     

Toughness Properties of a Silicon Carbide with an in Situ Induced Heterogeneous Grain Structure

Toughness characteristics of a heterogeneous silicon carbide with a coarsened and elongated grain structure and an intergranular second phase are evaluated relative to a homogeneous, fine-grain control using indentation–strength data. The heterogeneous material exhibits a distinctive flaw tolerance, indicative of a pronounced toughness curve. Quantitative evaluation of the data reveals an enhanced toughness in the long-crack region, with the implication of degraded toughness in the short-crack region. The enhanced long-crack toughness is identified with crack-interface bridging. The degraded short-crack toughness is attributed to weakened grain or interface boundaries and to internal residual stresses from thermal expansion mismatch. A profound manifestation of the toughness-curve behavior is a transition in the nature of mechanical damage in Hertzian contacts, from classical single-crack cone fracture in the homogeneous control to distributed subsurface damage in the heterogeneous material.     

Particle occlusion and mechanical properties of Ni–Al2O3 nanocomposites

Polycrystalline alumina, doped with MgO below the solubility limit, was reinforced with sub-micron particles of Ni by infiltration of Ni-nitrate into fired alumina green bodies, followed by reduction and sintering. The Ni particle size and location were monitored both after reduction and after sintering by transmission electron microscopy. Particle occlusion was found to increase with sintering time and temperature, and is correlated with experimentally detected Mg segregation to the Ni–alumina interfaces, resulting in partial depletion of Mg at the alumina grain boundaries and thus their increased mobility. Occlusion of Ni particles reduces the fracture strength and Weibull modulus of the composites, indicating that particle location is a key microstructural parameter for reaching high fracture strengths, and that this can be controlled via grain boundary and interface adsorption.     

Structure of Alumina Grain Boundaries Prepared with and without a Thin Amorphous Intergranular Film

The presence of a thin amorphous intergranular film along grain boundaries in alumina is expected to affect the properties of the interface and hence those of the material. In the present study, two types of grain boundaries have been formed in hot-pressed alumina bicrystals. In one case, the surfaces of the sintered crystals were kept as clean as possible, while in the other a thin layer of SiO₂ was intentionally deposited onto the surface of one crystal. The distribution of SiO₂ along the resulting grain boundary was then monitored by transmission electron microscopy and compared with the morphological features of the interface. In the special cases chosen here, the glass receded into large pores which grew into the alumina itself. However, the presence of the glassy phase during the early stages of sintering clearly did influence the characteristics of the resulting grain boundaries.     

The effect of rare earth dopants on grain boundary cohesion in alumina

The effect of rare earth (RE) grain boundary segregation on mode of fracture in alumina has been investigated. In order to isolate the effects of microstructure (i.e. grain size and residual porosity) from those due to grain boundary chemistry, the fracture behaviour of virtually pore-free (i.e. nearly transparent) undoped alumina has also been studied. This showed that mode of fracture becomes increasingly transgranular as grain size is reduced, a trend which has been explained by thermal expansion anisotropy effects.The addition of RE (i.e. Yb, Gd or La) dopants to alumina resulted in a substantial increase in the proportion of intergranular fracture relative to the undoped material of similar grain size. This can be explained by the significant reduction in the free surface energy that results from RE segregation at grain boundaries, which reduces the work of fracture for intergranular failure. This is expected to lead to a reduction in strength compared to undoped aluminas with equivalent microstructures, although this is often more than offset by the improved microstructures that using a RE dopant can provide.     

Creep Deformation of an Alumina Matrix Composite Reinforced with Silicon Carbide Whiskers

Whisker-reinforced ceramic composites with enhanced fracture toughness properties are being developed. The creep behavior of such a composite was studied. The introduction of silicon carbide whiskers significantly improves the creep resistance of polycrystaline alumina.