Reactive Hot Pressing of SiC/MoSi2 Nanocomposites

Dense SiC/MoSi₂ nanocomposites were fabricated by reactive hot pressing the mixed powders of Mo, Si, and nano-SiC particles coated homogeneously on the surface of Si powder by polymer processing. Phase composition and microstructure were determined by methods of X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and energy-dispersive spectrometry. The nanocomposites obtained consisted of MoSi₂, β-SiC, less Mo₅Si₃, and SiO₂. A uniform dispersion of nano-SiC particles was obtained in the MoSi₂ matrix. The relative densities of the monolithic material and nanocomposite were above 98%. The room-temperature flexural strength of 15 vol% SiC/MoSi₂ nanocomposite was 610 MPa, which increased 141% compared with that of the monolithic MoSi₂. The fracture toughness of the nanocomposite exceeded that of pure MoSi₂, and the 1200°C yield strength measured for the nanocomposite reached 720 MPa.     

Properties and Microstructure of Molybdenum Disilicide–β';-SiAlON Particulate Ceramic Composites

Particulate ceramic composites that were composed of a combustion-synthesized β';-SiAlON matrix and dispersed MoSi₂ particles were hot pressed at 1600°C in a nitrogen atmosphere. The physical and mechanical properties of the composites that contained 15, 30, and 45 vol% MoSi₂ were evaluated. The average four-point bend strength, fracture toughness, and Vickers hardness of the composites were in the ranges of 500-600 MPa, 3-4 MP·am^1/2, and 11-13 GPa, respectively. The measured mechanical strength and hardness were very similar to the values that were predicted from the rule of mixtures. The fracture toughness of the combustion-synthesized β';-SiAlON (2.5 MPa·m^1/2) was apparently enhanced by the MoSi₂ particles that were added. The increase in the fracture toughness was predominately attributed to the residual thermal stress that was induced by the thermal expansion mismatch between the MoSi₂ particles and the β';-SiAlON matrix. The composites showed improved electrical conductivity and oxidation resistance over monolithic β';-SiAlON. High-resolution transmission electron microscopy examination of the composites indicated that the MoSi₂ was chemically well compatible with the β';-SiAlON.     

Properties of Silicon Nitride–Molybdenum Disilicide Particulate Ceramic Composites

The physical and mechanical properties of hot-pressed Si₃N₄–MoSi₂ particulate composites containing 15 and 30 vol% MoSi₂ were studied. The average room-temperature four-point bend strength, fracture toughness, and electrical resistivity are 522 MPa, 3.6 MPa·√m, and 6.3 × 10⁵Χ·cm for the 15 vol% MoSi₂ composite, and 487 MPa, 5.3 MPa·√m, and 0.31 Ω·cm for the 30 vol% MoSi₂ composite. The mechanical properties of the composites are very close to those of hot-pressed Si₃N₄ ceramics. The high electrical conductivity of the 30 vol% MoSi₂ composite was attributed to the percolation effect of MoSi₂ particles. Parabolic oxidation behaviors were observed for the 30 vol% MoSi₂ composite during the 1200°C long-term oxidation experiments.     

Microstructure and Mechanical Properties of In Situ Produced TiC/TiB2/MoSi2 Composites

A novel microstructure of in situ produced TiC/TiB₂/MoSi₂ composite and its mechanical properties were investigated. The results indicate that TiC/TiB₂/MoSi₂ composites can be fabricated by reactive hot pressing the mixed powders of MoSi₂, B₄C, and Ti. A novel microstructure consisting of hollow particles of TiC and TiB₂ grains in an MoSi₂ matrix was obtained. Grains of in situ produced TiC and TiB₂ were much finer, from 100 to 400 nm. During the fracture process, hollow particles relieved crack tip stress, encouraging crack branching and changing the original direction of the main crack. The highest bending strength of this composite achieved was 480 MPa, twice that of monolithic MoSi₂, and the greatest fracture toughness of the composite reached 5.2 MPa·m^1/2.     

Reactive Hot Pressing of Alumina-Silicon Carbide Nanocomposites

A dense alumina-silicon carbide (Al₂O₃–SiC) nanocomposite was synthesized in situ from the reaction of mullite, aluminum, and carbon by reactive hot pressing (RHP). Transmission electron microscopy investigation showed that in situ -formed, nanometer-sized SiC particles were mainly entrapped in the matrix grains, whereas submicrometer-sized particles were located at the grain boundaries or triple points of the Al₂O₃. In addition, no amorphous phase was observed at the interfaces of the Al₂O₃ and SiC grains, which indicated strong direct bonding. Fracture-surface analysis by scanning electron microscopy revealed an intrafracture mode. The bending strength of the nanocomposite RHP-treated at 1800°C was 795 ± 160 MPa, and the fracture toughness, measured by the indentation method, was 3.1 MPa·m^1/2.     

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 Characterization of Three-Dimensional Carbon Fiber Reinforced Silicon Carbide and Silicon Nitride Composites

Three-dimensional (3D) carbon fiber reinforced SiC and Si₃N₄ composites have been fabricated using repeated infiltration of an organosilicon slurry under vacuum and pressure. Open porosity of the infiltrated body was reduced from 40% after the first infiltration to approximately 8% after the seventh cycle. Further reduction of open porosity to less than 3% was accomplished by hot-press densification. The maximum values of flexural strength and fracture toughness were, respectively, 260 MPa and 7.3 MPa·m^1/2for C/Si₃N₄ composites, and 185 MPa and 6 MPa·m^1/2 for C/SiC composite.     

Mechanical Behavior of Alumina–Silicon Carbide „Nanocomposites”

The fracture behavior of Al₂O₃ containing 5 vol% 0.15μm SiC particles was investigated using indentation techniques. A significant increase in strength was achieved by the addition of SiC particles to the base Al₂O₃. Specifically, the strength increased from 560 MPa for Al₂O₃ to 760 MPa for the composite samples (average values for unindented hotpressed bars tested in four-point bending). After annealing for 2 h at 1300°C, the average strength of the composite samples increased to about 1000 MPa. Toughness was estimated using indentation-strength data. While there was a slight increase in toughness, the increase was not sufficient to account for the increase in the unindented strength on SiC particle addition. It is suggested that the observed strengthening and apparent toughening were due to a machining-induced compressive surface stress.     

Properties of a Pressureless-Sintered ZrB2–MoSi2 Ceramic Composite

A ZrB₂-based composite was fully densified by pressureless sintering at 1850°C with addition of 20 vol% MoSi₂. The microstructure was very fine, with mean dimensions of ZrB₂ grains around 2.5 μm. The four-point flexural strength in air was in excess of 500 MPa up to 1500°C.     

Thermal and Electric Properties in Hot-Pressed ZrB2–MoSi2–SiC Composites

The thermal and electrical properties of MoSi₂ and/or SiC-containing ZrB₂-based composites and the effects of MoSi₂ and SiC contents were examined in hot-pressed ZrB₂–MoSi₂–SiC composites. The thermal conductivity and electrical conductivity of the ZrB₂–MoSi₂–SiC composites were measured at room temperature by a nanoflash technique and a current–voltage method, respectively. The results indicate that the thermal and electrical conductivities of ZrB₂–MoSi₂–SiC composites are dependent on the amount of MoSi₂ and SiC. The thermal conductivities observed for all of the compositions were more than 75 W·(m·K)⁻¹. A maximum conductivity of 97.55 W·(m·K)⁻¹ was measured for the 20 vol% MoSi₂-30 vol% SiC-containing ZrB₂ composite. On the other hand, the electrical conductivities observed for all of the compositions were in the range from 4.07 × 10–8.11 × 10 Ω⁻¹·cm⁻¹.     

Fabrication of Machinable Silicon Carbide-Boron Nitride Ceramic Nanocomposites

SiC/BN nanocomposite powders with the microstructure of micrometer-sized SiC particles coated with nanometer-sized BN particles were prepared via a chemical reaction, which used a mixture of boric acid (H₃BO₃) and urea (CO(NH₂)₂) as reactants coated on the surface of the SiC particles to react under a nitrogen-gas atmosphere. The results of XRD, TEM, and SAED studies showed that the coating layer (BN) was composed mostly of amorphous and nanometer-sized BN particles at the reaction temperature of 850°C. When the nanocomposite powders were hot-pressed at 1850°C, machinable SiC/BN ceramic nanocomposites with fine grain size and homogeneous microstructure were fabricated. The composite that contained 20 wt% BN exhibited high strength (the three-point bending strength was 588.4 ± 26.8 MPa) and excellent machinability.     

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.     

Properties of ZrB2–SiC Ceramics by Pressureless Sintering

Pressureless sintering was used to densify ZrB₂–SiC ultra-high temperature ceramics. The physical, mechanical, thermal, electrical, and high temperature properties were investigated. This comprehensive set of properties was measured for ZrB₂ containing 20 vol% SiC in which B₄C and C were used as the sintering aids. The three-point flexural strength was 361±44 MPa and the elastic modulus was 374±25 GPa. The Vickers hardness and fracture toughness were 14.7±0.2 GPa and 4.0±0.5 MPa·m^1/2 respectively. Scanning electron microscopy studies of the microstructure of ZrB₂–SiC showed that SiC particles were distributed homogenously in the ZrB₂ matrix with little residual porosity.     

Preparation, Microstructure, and Mechanical Properties of Silicon Carbide–Dysprosia Composites

Composites of silicon carbide (SiC) with up to 30 vol% of dysprosia (Dy₂O₃) were fabricated by hot pressing and hot isostatic pressing. The effects of Dy₂O₃ dispersions on the microstructure and on selected mechanical properties of the composites were investigated. When 10-15 vol% of Dy₂O₃ was dispersed in the SiC matrix, the fracture toughness increased by ∼40%, whereas the flexural strength was comparable to that of unreinforced SiC. The increased fracture toughness was due to crack deflection, in conjunction with crack-interface grain bridging, and was not related to a phase transformation of Dy₂O₃ in the matrix.     

Mechanical Behavior of MoSi2 Reinforced–Si3N4Matrix Composites

The mechanical behavior of MoSi₂ reinforced–Si₃N₄ matrix composites was investigated as a function of MoSi₂ phase content, MoSi₂ phase size, and amount of MgO densification aid for the Si₃N₄ phase. Coarse-phase MoSi₂-Si₃N₄ composites exhibited higher room-temperature fracture toughness than fine-phase composites, reaching values >8 MP·am^1/2. Composite fracture toughness levels increased at elevated temperature. Fine-phase composites were stronger and more creep resistant than coarse phase composites. Room-temperature strengths >1000 MPa and impression creep rates of ∼10⁻⁸ s⁻¹ at 1200°C were observed. Increased MgO levels generally were deleterious to MoSi₂-Si₃N₄ mechanical properties. Internal stresses due to MoSi₂ and Si₃N₄ thermal expansion coefficient mismatch appeared to contribute to fracture toughening in MoSi₂-Si₃N₄ composites.     

Silicon Nitride/Silicon Carbide Nanocomposite Materials: I, Fabrication and Mechanical Properties at Room Temperature

The fabrication of dense Si₃N₄/SiC nanocomposite materials that contained 2.5-30 wt% SiC via gas-pressure sintering and hot pressing was investigated. The SiC particles originated from admixed commercial SiC powders, SiCN powders produced by plasma synthesis, in situ reaction pyrolysis of carbon-coated Si₃N₄ particles, and pyrolysis of a polycarbosilazane-based SiCN precursor. Based on thermodynamic calculations, criteria for minimum liquid-phase decomposition during sintering were developed. The best sintering results were obtained for sintering cycles that observed this criteria. Materials that contained plasma-synthesized SiCN exhibited high strengths (835-995 MPa) and fracture toughness values (7.4-7.8 MPam^1/2) at room temperature. Post-sintering thermal treatments led to a strength reduction.     

Strengthening of Porous Alumina by Pulse Electric Current Sintering and Nanocomposite Processing

Porous Al₂O₃ and SiC–dispersed-Al₂O₃ (Al₂O₃/SiC) nanocomposites with improved mechanical properties were fabricated using pulse electric current sintering (PECS). Microstructures with fine grains and enhanced neck growth, as well as high fracture strength, could be achieved via PECS of Al₂O₃. The incorporation of fine SiC particles into an Al₂O₃ matrix significantly increased the fracture strength of porous Al₂O₃. Based on microstructural observations, it was revealed that the refinement of Al₂O₃ grains and neck growth occurred by PECS and nanocomposite processing.     

Reactive Hot Pressing of Alumina-Molybdenum Disilicide Composites

Al₂O₃-MoSi₂ composites were prepared by reactive hot pressing using molybdenum, aluminum, and mullite powders as precursors. The Gibbs free energy was highly negative for the composite-forming reaction, which indicated that the products were stable relative to the reactants. After the reaction, the composites had high relative density, ∼96%. Based on the composite-forming reaction, the composites should have contained 18 vol% MoSi₂ in an Al₂O₃ matrix. Scanning electron microscopy revealed that the MoSi₂ inclusions were elongated, with an average thickness of ∼5 μm and inclusion lengths that ranged from 5 to 50 μm. Average composite strength was 467 MPa, and toughness was 3.7 MPa·m^1/2.     

Reaction Bonding and Mechanical Properties of Mullite/Silicon Carbide Composites

Based on the RBAO technology, low-shrinkage mullite/SiC/ Al₂O₃/ZrO₂ composites were fabricated. A powder mixture of 40 vol% Al, 30 vol% A1₂O₃ and 30 vol% SiC was attrition milled in acetone with TZP balls which introduced a substantial ZrO₂ wear debris into the mixture. The precursor powder was isopressed at 300–900 MPa and heattreated in air by two different cycles resulting in various phase ratios in the final products. During heating, Al oxidizes to Al₂O₃ completely, while SiC oxidizes to SiO₂ only on its surface. Fast densification (at >1300°C) and mullite formation (at 1400°C) prevent further oxidation of the SiC particles. Because of the volume expansion associated with the oxidation of Al (28%), SiC (108%), and the mullitization (4.2%), sintering shrinkage is effectively compensated. The reaction-bonded composites exhibit low linear shrinkages and high strengths: shrinkages of 7.2%, 4.8%, and 3%, and strengths of 610, 580, and 490 MPa, corresponding to compaction pressure of 300, 600, and 900 MPa, respectively, were achieved in samples containing 49–55 vol% mullite. HIPing improved significantly the mechanical properties: a fracture strength of 490 MPa and a toughness of 4.1 MPa^.m^1/2 increased to 890 MPa and 6 MPa^.m^1/2, respectively.     

Toughening of Silicon Nitride Matrix Composites by the Addition of Both Silicon Carbide Whiskers and Silicon Carbide Particles

Si₃N₄ matrix composites reinforced by SiC whiskers, SiC particles, or both were fabricated using the hot-pressing technique. The mechanical properties of the composites containing various amounts of these SiC reinforcing materials and different sizes of SiC particles were investigated. Fracture toughness of the composites was significantly improved by introducing SiC whiskers and particles together, compared with that obtained by adding SiC whiskers or SiC particles alone. On increasing the size of the added SiC particles, the fracture toughness of the composites reinforced by both whiskers and particles was increased. Their fracture toughness also showed a strong dependence on the amount of SiC particles (average size 40 μm) and was a maximum at the particle content of 10 vol%. The maximum fracture toughness of these composites was 10.5 MPa·m^1/2 and the flexural strength was 550 MPa after addition of 20 vol% of SiC whiskers and 10 vol% of SiC particles having an average particle size of 40 μm. These mechanical properties were almost constant from room temperature to temperatures around 1000°C. Fracture surface observations revealed that the reinforcing mechanisms acting in these composites were crack deflection and crack branching by SiC particles and pullout of SiC whiskers.