Processing and Tribological Properties of Si3N4/Carbon Short Fiber Composites

Si₃N₄/carbon fiber composites were fabricated using several types of fiber. All the composites had higher fracture toughness compared with monolithic Si₃N₄ ceramics. Tribological properties were investigated by a ball-on-disk method under unlubricated conditions. The composite containing fibers with a high orientation of graphite layers and high graphite content indicated a low friction coefficient. It was identified, by Raman spectroscopy, that graphite was transferred from the composite to the Si₃N₄ ball of the counterbody during the wear test. This transferred layer was effective for producing the low friction behavior of the composite.     

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.     

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.     

Tribological Behavior of a Si3N4/Carbon Short Fiber Composite under Water Lubrication

The tribological behavior of monolithic Si₃N₄ and a Si₃N₄/carbon fiber composite has been assessed under high load and low speeds in an aqueous environment. The results showed that the friction coefficient of the Si₃N₄ was not significantly reduced when compared with dry sliding, and this was attributed to the failure to maintain a lubricating layer between the solid–solid surfaces. In the case of the composite, the initial high friction coefficient was reduced shortly after the beginning of the wear test and maintained a low value (about 0.03) throughout. This was attributed to the solid lubricating effect of the composite resulting in lower stress at the contact asperities, preventing the removal of the lubricating layer.     

Lubricated Rolling and Sliding Wear of a SiC-Whisker-Reinforced Si3N4 Composite against M2 Tool Steel

Mineral oil lubricated rolling and sliding wear of SiC whisker (SiC_w) reinforced Si₃N₄ composite and monolithic Si₃N₄ prepared identically against M2 tool steel were investigated using a cylinder-on-cylinder apparatus. Wear of this Si₃N₄ was higher than that of the composite. Wear of the steel against Si₃N₄ was also higher than that against the composite. Relatively larger scale microfracture occurred in the Si₃N₄ than in the composite; more pullout and microchipping of carbide particles were observed in the steel against Si₃N₄ than against the composite. Polishing of the worn surfaces of the steel occurred in both sliding and rolling tests. This was attributed to fine, hard wear debris circulating in the contact area. Spalling was observed in the steel sliding against Si₃N₄ but not in the steel sliding against the composite.     

Tribological Behavior of Mo5Si3-Particle-Reinforced Silicon Nitride Composites

The tribological behavior of Mo₅Si₃-particle-reinforced silicon nitride (Si₃N₄) composites was investigated by pin-on-plate wear testing under dry conditions. The friction coefficient of the Mo₅Si₃–Si₃N₄ composites and Si₃N₄ essentially decreased slowly with the sliding distance, but showed sudden increase for several times during the wear testing. The average friction coefficient of the Si₃N₄ decreased with the incorporation of submicrometer-sized Mo₅Si₃ particles and also as the content of Mo₅Si₃ particles increased. When the Mo₅Si₃–Si₃N₄ composites were oxidized at 700°C in air, solid-lubricant MoO₃ particles were generated on the surface layer. Oxidized Mo₅Si₃–Si₃N₄ composites showed self-lubricating behavior, and the average friction coefficient and wear rate of the oxidized 2.8 wt% Mo₅Si₃–Si₃N₄ composite were 0.43 and 0.72 × 10⁻⁵ mm³ (N·m)⁻¹, respectively. Both values were ∼30% lower than those for the Si₃N₄ tested in an identical manner.     

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.     

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.     

Tribological Properties of Unidirectionally Aligned Silicon Nitride

A silicon nitride ceramic with unidirectionally aligned β-Si₃N₄ elongated grains (UA-SN) was fabricated by sintering the extruded Si₃N₄ green body with a small amount of rodlike β-Si₃N₄ seed. The effect of anisotropy in microstructure on tribological properties was investigated, compared with a fine-grained Si₃N₄ without seed. Block-on-ring tests without lubricant were conducted at sliding speeds of 0.15 and 1.5 m/s, with a normal load of 5 N and a sliding distance of 75 m, using the UA-SN and Si₃N₄ without seeds as block specimens and commercially supplied Si₃N₄ as ring specimens. For UA-SN, tribological properties were evaluated in three directions with respect to the grain alignment: the plane normal to the grain alignment, and in the direction parallel to or perpendicular to the grain alignment in the side plane. For both sliding speeds, the plane normal to the grain alignment exhibited the highest wear resistance, and the worn surface of this plane was quite smooth, in contrast to the other specimens whose surfaces were irregular owing to grain dropping. It is considered that the high wear resistance achieved in this plane is attributable to the inhibition of crack propagation along the sliding surface by the stacked elongated grains normal to the sliding surface.     

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.     

Tribological Characteristics of Si3N4 Ceramic in High-Temperature and High-Pressure Water

The effects of sliding speed and dissolved oxygen on the tribological behavior of Si₃N₄ sliding on itself in water were investigated at room temperature and at 120°C saturated vapor pressure. The friction coefficients and specific wear rates at 120°C were much larger than those at room temperature and had a minimum at about 0.4 m/s, whereats -the specific wear rate of the disk increased with increasing the sliding speed. The wear rate at lower sliding speeds in water at 120°C is considered to be primarily controlled by the increase of the contact stress on the asperities which are formed by the dissolution of grain boundaries of the Si₃N₄ ceramic and the subsequent dissolution of the silica layer of the reaction product However, the wear rate at higher sliding speeds is governed by the direct oxidation and microfracture of the Si₃N₄ substrate. The tribochemical reaction to produce NH₃ mainly occurred at all sliding conditions in water at room temperature and 120°C, and the reaction to produce H₂ gas appeared slightly only at the sliding speeds above 0.4 m/s at 120°C. The tribological behavior was independent of dissolved oxygen concentration for all sliding conditions in water at room temperature and 120°C.     

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.     

Pressureless Sintering of Dense Si3N4 and Si3N4/SiC Composites with Nitrate Additives

The effect of aluminum and yttrium nitrate additives on the densification of monolithic Si₃N₄ and a Si₃N₄/SiC composite by pressureless sintering was compared with that of oxide additives. The surfaces of Si₃N₄ particles milled with aluminum and yttrium nitrates, which were added as methanol solutions, were coated with a different layer containing Al and Y from that of Si₃N₄ particles milled with oxide additives. Monolithic Si₃N₄ could be sintered to 94% of theoretical density (TD) at 1500°C with nitrate additives. The sintering temperature was about 100°C lower than the case with oxide additives. After pressureless sintering at 1750°C for 2 h in N₂, the bulk density of a Si₃N₄/20 wt% SiC composite reached 95% TD with nitrate additives.     

Elastic Properties of Al2O3 and Si3N4 Matrix Composites with SiC Whisker Reinforcement

A study of the elastic moduli of Al₂O₃ and Si₃N₄ ceramics reinforced with 0 to 25 wt% SiC whiskers has been performed. The Young's moduli, shear moduli, and longitudinal modulus are compared with calculated predictions for aligned fiber composites by Hill and Hashin and Rosen, and for fibers randomly oriented in three dimensions by Christensen and Waal. The measured values are in excellent quantitative agreement with those derived for the random orientation of the SiC whiskers.     

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.     

Fabrication and Microstructures of MoSi2 Reinforced–Si3N4 Matrix Composites

Details of the fabrication and microstructures of hot-pressed MoSi₂ reinforced–Si₃N₄ matrix composites were investigated as a function of MoSi₂ phase size and volume fraction, and amount of MgO densification aid. No reactions were observed between MoSi₂ and Si₃N₄ at the fabrication temperature of 1750°C. Composite microstructures varied from particle–matrix to cermet morphologies with increasing MoSi₂ phase content. The MgO densification aid was present only in the Si₃N₄ phase. An amorphous glassy phase was observed at the MoSi₂–Si₃N₄ phase boundaries, the extent of which decreased with decreased MgO level. No general microcracking was observed in the MoSi₂–Si₃N₄ composites, despite the presence of a substantial thermal expansion mismatch between the MoSi₂ and Si₃N₄ phases. The critical MoSi₂ particle diameter for microcracking was calculated to be 3 μm. MoSi₂ particles as large as 20 μm resulted in no composite microcracking; this indicated that significant stress relief occurred in these composites, probably because of plastic deformation of the MoSi₂ phase.     

Tribological Properties of a Zr2Al3C4 Ceramic at Ambient Temperature

In this work, reciprocating ball-on-flat sliding friction and wear tests as well as two-body abrasive wear tests were performed on Zr₂Al₃C₄, a new type of ceramic material. In the sliding wear tests, a Si₃N₄ ball and an AISI 52100 steel ball were used as counter materials. When Zr₂Al₃C₄ was slid against an AISI 52100 ball, the coefficient of friction (COF) was as low as 0.20–0.42, being independent of normal loads, and the wear rates of Zr₂Al₃C₄ and AISI 52100 steel were in the range of 10⁻⁴–10⁻⁵ mm³/m. A tribofilm between the tribopair was presumed to be responsible for the low COF and wear rate. According to Raman and energy-dispersive spectroscopy analysis, the tribofilm consists of a mixture of oxides of Zr, Al, and Fe as well as amorphous carbon. When Zr₂Al₃C₄ was slid against a Si₃N₄ ball, a transition from mild wear to severe wear was observed as the normal load increased. The transition occurs under certain contact stresses after a damage-accumulating period. In the two-body abrasive wear test, surface chipping and fragmentation resulting from coalescence of surface and subsurface microcracks were the main material removal mechanisms of Zr₂Al₃C₄.     

Comparison of Tribological Behavior Between α-Sialon/Si3N4 and Si3N4/Si3N4 Sliding Pairs in Water Lubrication

We report here the study on tribological behavior of α-Sialon in aqueous medium. The results derived from a wide range of test conditions are briefly discussed. A reduction in friction coefficient from 0.7 to 0.03 and a decrease in wear rate by two orders of magnitude were achieved under low load (9.8 N) and high speed (>0.54 m/s) conditions. The tribological behavior of α-Sialon/Si₃N₄ ceramics was then compared with Si₃N₄/Si₃N₄ tribopairs.     

Effect of Grain Size on the Thermal Conductivity of Si3N4

Polycrystalline Si₃N₄ samples with different grain-size distributions and a nearly constant volume content of grain-boundary phase (6.3 vol%) were fabricated by hot-pressing at 1800°C and subsequent HIP sintering at 2400°C. The HIP treatment of hot-pressed Si₃N₄ resulted in the formation of a large amount of ß-Si₃N₄ grains ∼10 µm in diameter and ∼50 µm long, and the elimination of smaller matrix grains. The room-temperature thermal conductivities of the HIPed Si₃N₄ materials were 80 and 102 Wm⁻¹K⁻¹, respectively, in the directions parallel and perpendicular to the hot-pressing axis. These values are slightly higher than those obtained for hot-pressed samples (78 and 93 Wm⁻¹K⁻¹). The calculated phonon mean free path of sintered Si₃N₄ was ∼20 nm at room temperature, which is very small as compared to the grain size. Experimental observations and theoretical calculations showed that the thermal conductivity of Si₃N₄ at room temperature is independent of grain size, but is controlled by the internal defect structure of the grains such as point defects and dislocations.     

Influence of Carbon Fiber Additions on Friction Properties and Running-In Behavior of Silicon Nitride-Based Composites Under Water Lubrication

The friction behavior of Si₃N₄/carbon fiber composites under various sliding conditions and with various carbon fiber contents was researched. The carbon fiber content did not affect the friction coefficient under hydrodynamic-type lubrication, but the running in distance decreased with increasing carbon fiber content. In a Stribeck analysis, the addition of carbon fibers to the Si₃N₄ material shifted the transition point from a hydrodynamic to mixed lubrication regime to more severe conditions, and had an effect on the friction coefficient under the boundary lubrication-type regime.