Use of Weibull Statistics to Correlate MOR, Ball-on-Ring, and Rotational Fast Fracture Tests

Fast fracture strength data on slip-cast reaction-bonded Si₃N₄ determined by uniaxial MOR, biaxial ball-on-ring tests, and speed of rotational failure measurements were correlated using Weibull statistics and finite-element techniques. The agreement between predicted and observed values demonstrated the applicability of the Weibull equation.     

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.     

Fabrication and Mechanical Properties of Si3N4/Carbon Fiber Composites with Aligned Microstructure Produced by a Seeding and Extrusion Method

Si₃N₄/carbon fiber composites have been produced with and without seeding by an extrusion and sintering process. In both cases the carbon fibers were aligned along the direction of extrusion, but the Si₃N₄ grains were only aligned in the seeded material. The mechanical properties of the specimens showed anisotropy with respect to the grain alignment, with both strength and toughness being highest in the direction parallel to the extruding direction. In this direction the seeded specimen, where both the Si₃N₄ grains and the carbon fibers were aligned, showed both higher fracture toughness and higher fracture strength than the nonseeded specimen where only the fibers were aligned.     

Fractography, Mechanical Properties, and Microstructure of Commercial Silicon Nitride–Titanium Nitride Composites

Commercial-grade Si₃N₄–TiN composites with 0, 10, 20, and 30 wt% TiN content have been characterized. Submicrometer grain-size Si₃N₄ was reinforced with fine TiN grains. Density, Young's modulus, coefficient of thermal expansion, and fracture toughness increased linearly with TiN content. Increased strength was observed in the Si₃N₄+20 wt% TiN, and Si₃N₄+30 wt% TiN composites. Fractography was used to characterize the different types of fracture origins. Improvements in toughness and strength are due to residual stresses in the Si₃N₄ matrix and the TiN particles. A threefold improvement in dry wear resistance of the Si₃N₄+30 wt% TiN composite over the Si₃N₄ matrix was observed.     

Relation Between Strength, Fracture Energy, and Microstructure of Hot-Pressed Si3N4

A fracture mechanics approach was used to investigate the high strength of hot-pressed Si₃N₄. Room-temperature flexural strengths, fracture energies, and elastic moduli were determined for material fabricated from α- and β-phase Si₃N₄ powders. When the proper powder preparation technique was used, α-phase powder resulted in a high fracture energy (69,000 ergs/cm²), a high flexural strength (95,000 psi), and an elongated (fiberlike) grain morphology, whereas β-phase powder produced a low fracture energy (16,000 ergs/cm²), a relatively low strength (55,000 psi), and an equiaxed grain morphology. It was hypothesized that the high strength of Si₃N₄ hot-pressed from α-phase powder results from its high fracture energy, which is attributed to the elongated grains. High-strength Si₃N₄ has directional properties caused, in part, by the elongated grain structure, which is oriented preferentially with respect to the hot-pressing direction.     

Microstructural Characterization and Mechanical Properties of Si3N4 Formed by Fused Deposition of Ceramics

We present processing (green and sintered), part shrinkage and warping, microstructural characterization, and mechanical properties of Si₃N₄ made by fused deposition of ceramics (FDC), using optical microscopy, scanning electron microscopy, and X-ray diffraction. The mechanical properties (fracture strength, fracture toughness, and Weibull modulus) are also reported. Proper FDC build parameters resulted in dense, homogeneous, near-net-shape Si₃N₄, with microstructures and mechanical properties similar to conventionally processed material. Mechanical properties are shown to be isotropic, while there is some degree of microstructural texturing (preferred β-Si₃N₄ grain orientation) in sintered components.     

High-Temperature Failure Mechanisms of Hot-Pressed Si3N4 and Si3N4/Si3N4-Whisker-Reinforced Composites

The high-temperature flexural strength of hot-pressed silicon nitride (Si₃N₄) and Si₃N₄-whisker-reinforced Si₃N₄-matrix composites has been measured at a crosshead speed of 1.27 mm/min and temperatures up to 1400°C in a nitrogen atmosphere. Load–displacement curves for whisker-reinforced composites showed nonelastic fracture behavior at 1400°C. In contrast, such behavior was not observed for monolithic Si₃N₄. Microstructures of both materials have been examined by scanning and transmission electron microscopy. The results indicate that grain-boundary sliding could be responsible for strength degradation in both monolithic Si₃N₄ and its whisker composites. The origin of the nonelastic failure behavior of Si₃N₄-whisker composite at 1400°C was not positively identified but several possibilities are discussed.     

Reaction-Bonded and Superplastically Sinter-Forged Silicon Nitride–Silicon Carbide Nanocomposites

Silicon nitride–silicon carbide (Si₃N₄–SiC) nanocomposites were fabricated by a process involving reaction bonding followed by superplastic sinter-forging. The nanocomposites exhibited an anisotropic microstructure, in which rod-shaped, micrometer-sized Si₃N₄ grains tended to align with their long axes along the material-flow direction. SiC particles, typically measuring several hundred nanometers, were located at the Si₃N₄ grain boundaries, and nanosized particles were dispersed inside the Si₃N₄ grains. A high bending strength of 1246 ± 119 MPa, as well as a high fracture toughness of 8.2 ± 0.9 MPa·m^1/2, was achieved when a stress was applied along the grain-alignment direction.     

Evaluation of Brazed Silicon Nitride Joints: Microstructure and Mechanical Properties

Sintered Si₃N₄ has been bonded to itself and to AISI 316 steel by the active-metal brazing route. A commercial Ag-35Cu-1.6Ti filler has been used with joining taking place during a 30 min hold at 850°C under vacuum. Si₃N₄/ Si₃N₄ joints have been produced with strength distribution (average bend strength = 773.5 MPa, Weibull modulus = 11.2) similar to that of the monolithic ceramic. Direct brazing of the Si₃N₄ to AISI 316 steel was unsuccessful. However, reliably strong (bend strength of 250–400 MPa) ceramic/ steel joints with 20 × 20 mm² cross sections were fabricated by using Cu, Mo, or Nb interlayers. The most potent inter-layer used in this work was Mo, whose coefficient of thermal expansion matches best that of the ceramic.     

Machinability of Silicon Nitride/Boron Nitride Nanocomposites

The machinability and deformation mechanism of Si₃N₄/BN nanocomposites were investigated in the present work. The fracture strength of Si₃N₄/BN microcomposites remarkably decreased with increased hexagonal graphitic boron nitride ( h -BN) content, although machinability was somewhat improved. However, the nanocomposites fabricated using the chemical method simultaneously had high fracture strength and good machinability. Hertzian contact tests were performed to clarify the deformation behavior by mechanical shock. As a result of this test, the damage of the monolithic Si₃N₄ and Si₃N₄/BN microcomposites indicated a classical Hertzian cone fracture and many large cracks, whereas the damage observed in the nanocomposites appeared to be quasi-plastic deformation.     

Fracture Energies of Tape-Cast Silicon Nitride with β-Si3N4 Seed Addition

The fracture energies of the tape-cast silicon nitride with and without 3 wt% rod-like β-Si₃N₄ seed addition were investigated by a chevron-notched-beam technique. The material was doped with Lu₂O₃–SiO₂ as sintering additives for giving rigid grain boundaries and good heat resistance. The seeded and tape-cast silicon nitride has anisotropic microstructure, where the fibrous grains grown from seeds were preferentially aligned parallel to the casting direction. When a stress was applied parallel to the fibrous grain alignment direction, the strength measured at 1500°C was 738 MPa, which was almost the same as room temperature strength 739 MPa. The fracture energy of the tape-cast Si₃N₄ without seed addition was 109 and 454 J/m² at room temperature and 1500°C, respectively. On the contrary, the fracture energy of the seeded and tape-cast Si₃N₄ was 301 and 781 J/m² at room temperature and 1500°C, respectively, when a stress was applied parallel to the fibrous gain alignment. The large fracture energies were attributable primarily to the unidirectional alignment fibrous Si₃N₄ grains.     

Crack-Healing Behavior of Si3N4/SiC Ceramics under Cyclic Stress and Resultant Fatigue Strength at the Healing Temperature

Si₃N₄/SiC composite ceramics were sintered and subjected to three-point bending. A semi-elliptical surface crack of 100 μm surface length was made on each specimen. The crack-healing behavior under cyclic stress of 5 Hz, and resultant cyclic fatigue strengths at healing temperatures of 1100° and 1200°C, were systematically investigated. The main conclusions are as follows: (1) Si₃N₄/SiC composite ceramics have an excellent ability to heal a crack at 1100° and 1200°C. (2) This sample could heal a crack even under cyclic stress at a frequency of 5 Hz. (3) The crack-healed sample exhibited quite high cyclic fatigue strength at each crack-healing temperature, 1100° and 1200°C.     

Water-Based Gelcasting of Surface-Coated Silicon Nitride Powder

A layer of Y₂O₃–Al₂O₃, used as a sintering aid, was coated onto the surface of Si₃N₄ particles by the precipitation of inorganic salts from a water-based solution containing Al(NO₃)₃, Y(NO₃)₃, and urea. The electrokinetic and colloidal characteristics of the Si₃N₄ powder were changed significantly by the coating layer. As a result, dispersion of the Y₂O₃–Al₂O₃-coated Si₃N₄ powder was significantly greater than that of the original powder. Furthermore, the Y₂O₃–Al₂O₃ coating layer prevented the hydrogen-gas-discharging problem that occurred during gelcasting of the original Si₃N₄ powder because of reaction between the uncoated powder and the basic aqueous solution in suspension. Surface coating, as well as the gelcasting process, significantly improved the microstructure, room-temperature bending strength, and Weibull modulus of the resulting ceramic bodies.     

Tribological Behavior of Si3N4 and Si3N4/Carbon Fiber Composites Against Stainless Steel Under Water Lubrication for a Thrust-Bearing Application

The tribological behavior of Si₃N₄ ceramics and Si₃N₄/carbon fiber composites sliding against stainless steel under water lubrication was investigated using a thrust-bearing-type test method with normal applied loads varying from 0 to 1000 N in 100 N increments. In the case of the monolithic Si₃N₄, the friction coefficient was found to increase up to 0.4 the first time the applied load was increased from 100 to 200 N, and sudden failure of the ceramic ring specimen occurred. In the case of the Si₃N₄/carbon fiber composite, a low friction coefficient was maintained up to the maximum normal load of 1000 N. The addition of the carbon fibers to the silicon nitride ceramics effectively restricts material transfer from the stainless steel to the Si₃N₄ worn surface due to reduction of solid–solid contact through the solid lubricating effect of the carbon fibers.     

Atomistic Structure of Silicon Nitride/Silicate Glass Interfaces

The structure of interfaces formed by a Si₃N₄ grain and the silica-rich intergranular amorphous phase was investigated by quantitative high-resolution transmission electron microscopy (QHRTEM). It was found that the contrast and periodicity of the HRTEM image of β-Si₃N₄ strongly depend on the specimen thickness and objective lens focus value. The different thinning rate between Si₃N₄ and the glass phase during ion-milling results in gradients of the specimen thickness at the interfaces. The interface roughness can also lead to a thickness variation of Si₃N₄ near the interface parallel to the electron beam. As a result, the HRTEM micrographs, taken from the thin specimen regions near the interfaces at a certain defocus value, show the occurrence of an artifact of an ordered structure seemingly different from Si₃N₄. The present investigations, however, showed that no ordered phase actually different from that of Si₃N₄ at the interfacial region in Si₃N₄ could be identified so far. The interfacial structure is likely direct Si₃N₄/glass bonding, rather than an ordered transition phase between the Si₃N₄ and the glass phase.     

Silicon Carbide Monofilament-Reinforced Silicon Nitride or Silicon Carbide Matrix Composites

SiC-monofilament-reinforced SiC or Si₃N₄ matrix composites were fabricated by hot-pressing, and their mechanical properties and effects of filaments and filament coating layers were studied. Relationships between frictional stress of filament/matrix interface and fracture toughness of SiC monofilament/Si₃N₄ matrix composites were also investigated. As a result, it was confirmed experimentally that in the case of composites fractured with filament pullout, the fracture toughness increased as the frictional stress increased. On the other hand, when frictional stress was too large (>about 80 MPa) for the filament to be pulled out, fracture toughnesses of the composites were almost the same and not so much improved over that of Si₃N₄ monolithic ceramics. The filament coating layers were found to have a significant effect on the frictional stress of the SiC monofilament/Si₃N₄ matrix interface and consequently the fracture toughness of the composites. Also the crack propagation behavior in the SiC monofilament/Si₃N₄ matrix composites was observed during flexural loading and cyclic loading tests by an in situ observation apparatus consisting of an SEM and a bending machine. The filament effect which obstructed crack propagation was clearly observed. Fatigue crack growth was not detected after 300 cyclic load applications.     

Effect of Silicon Carbide Whisker and Titanium Carbide Particulate Additions on the Friction and Wear Behavior of Silicon Nitride

A Si₃N₄/TiC composite was previously demonstrated to exhibit improved wear resistance compared to a monolithic Si₃N₄ because of the formation of a lubricious oxide film containing Ti and Si at 900°C. Further improvements of the composite have been made in this study through additions of SiC whiskers and improved processing. Four materials—Si₃N₄, Si₃N₄/TiC, Si₃N₄/SiC_wh, and Si₃N₄/TiC/SiC_wh— were processed to further optimize the wear resistance of Si₃N₄ through improvements in strength, hardness, fracture toughness, and the coefficient of friction. Oscillatory pin on flat wear tests showed a decrease in the coefficient of friction from ∼0.7 (Si₃N₄) to ∼0.4 with the addition of TiC at temperatures reaching 900°C. Wear track profiles illustrated the absence of appreciable wear on the TiC-containing composites at temperatures above 700°C. Microscopic (SEM) and chemical (AES) characterization of the wear tracks is also included to deduce respective wear and lubricating mechanisms.     

Influence of Planetary High-Energy Ball Milling on Microstructure and Mechanical Properties of Silicon Nitride Ceramics

The influence of ball-milling methods on microstructure and mechanical properties of silicon nitride (Si₃N₄) ceramics produced by pressureless sintering for a sintering additive from MgO–Al₂O₃–SiO₂ system was investigated. For planetary high-energy ball milling, the mechanical properties of Si₃N₄ ceramics were evidently improved and a homogeneous microstructure developed. In contrast, some exaggerated elongated grains were developed due to the local enrichment of sintering additives in the specimen prepared by general ball milling. For Si₃N₄ ceramics produced by planetary ball milling, flexure strength of 1.06 GPa, Vickers hardness of 14.2 GPa, and fracture toughness of 6.6 MPa·m^0.5 were achieved. The differences in the mechanical properties of Si₃N₄ ceramics produced by different processing seem to arise mainly from the changes in microstructural homogenization and sinterability. The planetary high-energy ball-milling process provides a good route to mix starting powders for developing ceramics with uniform microstructure and promising mechanical properties.     

Relationship between Microstructure and Mechanical Performance of a 70% Silicon Nitride–30% Barium Aluminum Silicate Self-Reinforced Ceramic Composite

The abnormal grain growth of β-Si₃N₄ was observed in a 70% Si₃N₄–30% barium aluminum silicate (70%-Si₃N₄–30%-BAS) self-reinforced composite that was pressureless-sintered at 1930°C; Si₃N₄ starting powders with a wide particle-size distribution were used. The addition of coarse Si₃N₄ powder encouraged the abnormal growth of β-Si₃N₄ grains, which allowed microstructural modification through control of the content and size distribution of β-Si₃N₄ nuclei. The mechanical response of different microstructures was characterized in terms of flexural strength, as well as indentation fracture resistance, at room temperature. The presence of even a small amount of abnormally grown β-Si₃N₄ grains improved the fracture toughness and minimized the variability in flexural strength.     

Abrasive Wear Behavior of a Si3N4-MoSi2 Composite

MoSi₂ particles (20 vol%) have been added to Si₃N₄ to form ceramic matrix-intermetallic composites. Benefits associated with the addition of the MoSi₂ to Si₃N₄ include higher strength, higher fracture toughness, no loss in oxidation resistance, and lower electrical resistivity. However, because the hardness of MoSi₂ is approximately half that of Si₃N₄, a decrease in the specific wear rate of the Si₃N₄-20 vol% MoSi₂ composite is expected to result from the incorporation of the MoSi₂ into the Si₃N₄. In this U.S. Bureau of Mines and Los Alamos National Laboratory study, it is found, however, that the specific wear rate of the composite during two-body abrasion by SiC particles is equivalent in magnitude to the specific wear rate of monolithic Si₃N₄. The specific wear rates of both the Si₃N₄-20 vol% MoSi₂composites and monolithic Si₃N₄ are four to five times less than that of monolithic MoSi₂.