Mechanical properties of Al2O3 particle-Y-TZP matrix composite and its toughening mechanism

Dense Al₂O₃ particle-Y-TZP matrix (Al₂O₃<40 vol%) composite was prepared by pressureless sintering at 1550°C. Composites with 10–30 vol% Al₂O₃ particles showed enhanced fracture toughness, bending strength and Vicker's hardness as compared to single-phase Y-TZP. The highest strength (1150 MPa) and highest toughness (12.4 MPa m^1/2) were obtained for the composite containing 10 vol% Al₂O₃. It was found that, in addition to the contribution by the crack-deflection effect, the enhanced phase transformation from tetragonal to monoclinic during fracture was the main toughening mechanism in operation in the composites.     

Effects of copper addition on the sintering behavior and mechanical properties of powder processed Al/SiC<Subscript><Emphasis Type="Bold">p</Emphasis></Subscript> composites

The effect of copper addition on powder processed Al-10 vol% SiC composites was studied in regards to their sintering responses. Copper was mixed with aluminum powder either as elemental powders or as the coated layer on SiC particles. After sintering at 600°C for 1 h, Al-SiC composites with no copper addition showed little densification. It also demonstrated very low bend strengths of 49 and 60 MPa, indicating poor bonding between the powders in the sintered composite. The addition of 8% copper to the Al/SiC system effectively improved the sintering response, producing over 95% theoretical density, a bend strength of 231 MPa with the copper coated SiC, and a 90% density with over 200 MPa bend strength with the admixed copper.The as-sintered microstructures of the Al–SiC composites clearly revealed particle boundaries and sharp pores, indicating that only a limited neck growth occurred during sintering. In the case of Al–Cu–SiC composites, however, a liquid phase was formed and spread through particle boundaries filling the interfaces or voids between SiC particles and the matrix powders. The coated copper on SiC particles produced a somewhat better filling of the interface or voids, resulting in a little more densification and better sintered strength. Since the solubility of copper in aluminum is less than 2% at the sintering temperature, the alloying of copper in the aluminum matrix was limited. Most of the copper added was dissolved in the liquid phase during the sintering and precipitated as CuAl₂ phase upon cooling.     

Preparation and characterization of lanthanum zirconate

Lanthanum zirconate has been prepared by citrate synthesis, by coprecipitation and by solid state decomposition of metal nitrate–urea mixtures. The relative advantages of these methods with respect to surface area and reproducibility are investigated. The lanthanum zirconate phase is formed by the urea decomposition method without any additional heat treatment. In the case of the citrate and coprecipitation methods the pyrochlore phase is formed only after heating the precursor above 900 °C. The citrate method yields the highest surface area, the coprecipitation method gives more reproducible results. However, after washing with ethanol the coprecipitated sample has much higher surface area compared with the citrate method. © 1998 Kluwer Academic Publishers     

Whisker reinforcement of glass-ceramics

Silicon carbide whisker reinforcement of anorthite and cordierite glass ceramics has been studied. At 25 vol% whisker loading the flexural strengths increased from 65–103 MPa to 380–410 MPa, the fracture toughnesses increased from 1.0–1.5 MPa m^1/2 to 5.2–5.5 MPa m^1/2. The strengths decline to 240–276 MPa at 1200 °C. The reasons for the decrease in strength with temperature are discussed. Whiskers from two different sources with differences in diameters and aspect ratios were evaluated and the effect of the whisker morphology on the composite properties was studied. It was found that larger diameter, higher aspect ratio whiskers result in improved composite performance. The composites were also characterized in terms of their thermal properties, i.e. thermal expansions and thermal conductivities. The thermal expansion coefficient from 25–1000 °C for anorthite-based composite was 4.6×10^–6 °C^–1 and that for the cordierite-based composite was 3.62×10^–6 °C^–1. The thermal conductivities at 1000 °C were 3.75 and 4.1 Wm^–1 K^–1 for cordierite and anorthite composites, respectively.     

Hot-pressed AlN-Cu metal matrix composites and their thermal properties

AlN-Cu metal matrix composites containing AlN volume fractions between 0.1 and 0.5 were fabricated firstly by liquid phase sintering of AlN using Y₂O₃ as a sintering aid and then by hot pressing the powder mixtures of sintered AlN and Cu at 1050°C with a pressure of 40 MPa under flowing nitrogen. With Y₂O₃ additions of 1.5 to 10 wt%, the densification of AlN could be achieved by liquid phase sintering at 1900°C for 3 h and subsequently slow cooling. The sintered AlN showed a maximum thermal conductivity of 166 W/m/K at a Y₂O₃ level of 6 wt%. Dense AlN-Cu composites with AlN contents up to 40 vol% were achieved by hot pressing. The thermal conductivity and the coefficient of the thermal expansion (CTE) of the composites decreased with increasing AlN volume fractions, giving typical values of 235 W/m/K and 12.6 × 10^–6/K at an AlN content of 40 vol%.     

Fe-based metallic glass particles reinforced Al-7075 matrix composites prepared by spark plasma sintering

Metallic glass (MG) reinforced aluminum matrix composites (AMCs) have attracted the interest of many researchers in the past few years. In this study, Fe₅₀Cr₂₅Mo₉B₁₃C₃ metallic glass (FMG) particles reinforced 7075 aluminum matrix (Al-7075) composites were prepared by spark plasma sintering (SPS) technique. The microstructure of the composites showed good interface bonding between the FMG particles and the matrix. The micro-hardness of the composite with 30 vol% FMG particles reached 160.63 HV, which was increased by 30% compared with that of Al-7075 (119.3 HV). The ultimate compression strength (UCS) of the composite was also improved significantly from 596 MPa for Al-7075 matrix to 749 MPa for the composite reinforced with 30 vol% FMG particles, and the compression strain of the composite reached 22%. These results indicate that the mechanical properties of the composites can be enhanced by adding high volume fraction FMG particles. The enhancement of the strength is resulted from multiple strengthening mechanisms, and the main contributions come from the thermal mismatch and grain refinement.     

The microstructure and elevated temperature strength of tungsten-titanium carbide composite

A new tungsten matrix composite containing 30 vol% titanium carbide particles (W-TiC) produced by sintering under 20 MPa pressure at 2000°C in a vacuum has been developed in order to improve the elevated temperature strength of tungsten. Flexural strength tests of the W-TiC composite in the temperature range 20–1200°C showed that the strength was significantly increased by the presence of TiC particles. The flexural strength at 1000°C was 1155 MPa, which was much higher than that at 20°C (770 MPa). Microstructural observations showed that a interdiffusion zone was produced at the W matrix-TiC particle interface, and a strong bond was formed between TiC and W, which was very beneficial to the elevated temperature mechanical properties. The mechanisms of fracture at 20°C and 1000°C were investigated. The fracture at 20°C was brittle. There was a growth-coalescence process for the initial cracks during the fracture process of the W-TiC composite at 1000°C, and the W matrix exhibited ductile tearing. The excellent elevated temperature strength of W-TiC composite was attributed to the brittle-ductile transition in the W matrix, which allows more effective strengthening from TiC particles.     

Liquid-phase sintering of chemically unstable silicon carbide-lithium/magnesium aluminosilicate-titania composites

The fully dense 55 wt % SiC-45 wt % (LAS/MAS/TiO₂) composite consisting of SiC filler particles and glassy matrix has been prepared by liquid-phase sintering in the presence of carbon, using the heating rate of 800C min^–1, the maximum sintering temperature 1600C and the nitrogen overpressure of 8×10^–5 Pa applied at a maximum particle mobility stage. The total liquid-phase sintering time did not exceed 4 min. The bloating effect was always observed in the carbon-free atmosphere during liquid-phase sintering.     

Fabrication process and thermal properties of SiCp/Al metal matrix composites for electronic packaging applications

The fabrication process and thermal properties of 50–71 vol% SiC_p/Al metal matrix composites (MMCs) for electronic packaging applications have been investigated. The preforms consisted with 50–71 vol% SiC particles were fabricated by the ball milling and pressing method. The SiC particles were mixed with SiO₂ as an inorganic binder, and cationic starch as a organic binder in distilled water. The mixtures were consolidated in a mold by pressing and dried in two step process, followed by calcination at 1100 °C. The SiC_p/Al composites were fabricated by the infiltration of Al melt into SiC preforms using squeeze casting process. The thermal conductivity ranged 120–177 W/mK and coefficient of thermal expansion ranged 6–10 × 10^–6/K were obtained in 50–71 vol% SiC_p/Al MMCs. The thermal conductivity of SiC_p/Al composite decreased with increasing volume fraction of SiC_p and with increasing the amount of inorganic binder. The coefficient of thermal expansion of SiC_p/Al composite decreased with increasing volume fraction of SiC_p, while thermal conductivity was insensitive to the amount of inorganic binder. The experimental values of the coefficient of thermal expansion and thermal conductivity were in good agreement with the calculated coefficient of thermal expansion based on Turner's model and the calculated thermal conductivity based on Maxwell's model.     

Fabrication and plastic deformation of Y-TZP/alumina nanocomposite ceramics containing oxynitride glass

Dense yttria-stabilized tetragonal zirconia polycrystals (Y-TZP) +28 vol% alumina nanocomposite ceramics with and without 17 vol% oxynitride glass were fabricated at 1380°C using microwave sintering. The specimens were uniaxially compressed in the temperature range 1250 to 1400°C. Strain rates as high as 10^–4 (s^–1) were measured at 1350°C and 90 MPa in the glass-free specimens with the stress exponent of 1.5. Similar strain rates were measured at lower compressive stresses in the counterpart glass-containing specimens. The stress exponent in the glass-containing specimens changed from 1.0 at 1250°C to 2.0 at higher temperatures. Dynamic grain growth of the alumina grains was inhibited in the presence of the oxynitride glass. Plastic deformation at lower temperatures in glass-containing alloy occurred by cooperative grain boundary sliding, aided by viscous flow of the grain boundary glassy phase. The changes in the deformation behavior at higher temperatures were related to crystallization of the glass and simultaneous plastic deformation by grain boundary sliding.     

Dielectric studies of PZT-polymer composites

Lead zirconate titanate (PZT)/Nylon 66 composites having 3-3 connectivity have been prepared by a relatively simple fabrication process. The d.c. conductivity and dielectric constant were measured from 30 to 220° C at various frequencies (0.1, 1, 10, 100 kHz). The dielectric constant increased with increasing temperature and PZT-constant of the composite up to 50 vol% PZT, but later showed a decrease due to increase in porosity in the samples. The dielectric constant also increased rapidly at higher temperature (> 100°C) for lower frequencies (0.1 and 1 kHz) due to intergrain polarization. The dielectric loss increased with increasing temperature and with decreasing PZT content of the composite. D.c. conductivity increased continuously with increasing temperature.     

Preparation and properties of SiO2 matrix composites doped with AlN particles

SiO₂ matrix composites doped with AlN particles were prepared by hot-pressing process. Mechanical properties of SiO₂ matrix composites can be greatly improved by doping with AlN particles. Flexural strength and fracture toughness of 30 vol%AlN-SiO₂ composite sintered at 1400°C reached 200 MPa and 2.96 MPa·m^1/2. XRD analysis indicated that, up to 1400°C, no chemical reaction occurred between SiO₂ matrix and AlN particles suggesting an excellent chemical compatibility of SiO₂ matrix with AlN particles. The influences of hot-pressing temperature and the content of AlN particles on dielectric properties of SiO₂-AlN composites were studied. The temperature and frequency dependency of dielectric properties of SiO₂-AlN composites were also studied. Residual flexural strength of SiO₂-AlN composites decreased with increasing temperature difference. The critical temperature difference was estimated about 600°C.     

Densification and microstructure development during the sintering of submicrometre magnesium oxide particles prepared by a vapour-phase oxidation process

The densification behaviour and microstructure development of MgO compacts fired from room temperature up to 1700°C at a heating rate of 10°C min^–1 were examined. Starting materials were seven kinds of MgO powder with primary particle sizes ranging from 11–261 nm; these powders were produced by a vapour-phase oxidation process. The original powders contained agglomerates, due to the spontaneous coagulation of primary particles, which ranged in size from 100–500 nm. The MgO compacts densified during firing by three types of sintering: sintering within agglomerates; sintering between agglomerates and grains; and rearrangement of agglomerates and grains. The MgO compact with the lowest primary particle size (11 nm) densified by the first and second types of sintering, but the effects of these two types of sintering decreased when the primary particle size became 44 nm; here the rearrangement of agglomerates and grains primarily contributed to densification of the compact. All three types of densification became less complete with further increases in primary particle size up to 261 nm. The relative densities of the MgO compacts with smaller primary particle sizes (11–44 nm) became 96–98% when the compacts were fired up to 1700°C.     

Microstructure and mechanical properties of silicon carbide fibre-reinforced aluminium nitride composite

SiC continuous fibre (15 vol%)/AlN composite was fabricated using a sintering additive of 4Ca(OH)₂ · Al₂O₃ by hot-pressing at 1650 °C and 17.6 MPa in vacuum. Analytical transmission electron microscopy and scanning electron microscopy were used to investigate the microstructure of as-fabricated and crept SiC fibre/AlN composites. The room-temperature mechanical and high-temperature creep properties of the composite were investigated by four-point bending. The incorporation of SiC fibre into AlN matrix improved significantly the room-temperature mechanical properties. This improvement could result from the crack deflections around the SiC fibres. However, the incorporation degraded severely the high-temperature creep properties under oxidizing atmosphere. This could be attributed to the development of the pores and various oxides at the matrix grain boundary and matrix/fibre interface during creep test.     

Organic-templating approach to synthesis of nanoporous silica composite membranes (l): TPA-templating and CO2 separation

Nanoporous silica composite membranes for gas separation have been synthesized by dip-coating the tetrapropylammonium (TPA)-templating silica sols on tubular alumina supports (pore size 2.8–100 nm), followed by eliminating the template via heat-treating at 550–600°C. The NMR spectroscopy of TPABr-silica hybrid composites obtained from the templated silica sols confirmed that TPA molecules (i.e., final pores) were uniformly distributed in the silica matrix. The average pore size and the specific surface area of an unsupported membrane prepared by firing the TPABr (6 wt%)-silica hybrid composite at 600°C were below 18 Å and 830 m²/g, respectively. Any defects such as cracks or pin-holes on the surface of amorphous silica composite membranes were not observed. The CO₂/N₂ separation factor of their composite membranes varied from 3.2 to 10.3 and their gas permeability from 10^–8 to 10^–9 mol/m² · s · Pa depending on the microstructure of aluminar supports.     

Properties of composites of 2014 aluminium alloy with Ni-Mo-based metallic glass particles

Composites of 2014 aluminium alloy containing dispersions of metallic glass particles (51.5wt% Ni, 38.0wt% Mo, 8.0wt% Cr and 1.5wt% B) have been prepared by a conventional powder metallurgy route involving powder mixing, compaction, sintering and heat treatment. Physical and mechanical properties of the composites, such as dimensional changes, hardness, electrical resistivity and corrosion behaviour, were studied. Dimensional growth up to a maximum of 6% in a linear direction was observed in all sintered composites. HardnessHv increased from 40 to 55kgmm^–2 with the addition of 4vol% of dispersoid, followed by a gradual decrease with increasing additions of dispersoid. The decrease in hardness above 4vol% of dispersoid was attributed to the presence of increasing amounts of porosity. Electrical resistivity increased from 50nm (for 2014 aluminium alloy) to 180nm at 20vol% dispersoid. The corrosion rate in an artificial sea water environment decreased linearly with the volume fraction of dispersoid. Re-pressing and re-sintering (in an argon atmosphere) of composites containing 4vol% of metallic glass particles resulted in an increase inHv from 55 (argon sintering) to 83kgmm^–2, and a decrease in electrical resistivity from 57 to 52nm due to the increase in density. The corrosion rate in an artificial sea water environment of composites containing 4vol% of metallic glass decreased from 70×10^–3 to 50×10^–3 mgdm^–2 per day due to re-pressing and re-sintering.     

A quantitative evaluation of microstructure in Si3N4/SiC platelet and participate composites

A microstructural evaluation of Si₃N₄ containing 15–40 vol% SiC platelets or particles is presented. All the composites were fully densified by hot isostatic pressing without external addition of sintering aids. Size, morphology, surface roughness and crystal structures of the SiC phases before and after sintering were compared in order to discuss the structural stability of the reinforcements up to 2050 °C in Si₃N₄ matrix. Morphology and phase characteristics of the grain boundary are also discussed. In addition, homogeneity and isotropy of the composite bodies were quantitatively examined by image analysis techniques and it was recognized that, for a similar degree of dispersion, the characteristic of three-dimensional randomness could be preserved only at V _f<30% in the composites containing high aspect ratio platelets.     

Silicon carbide fibre reinforced glass-ceramic matrix composites exhibiting high strength and toughness

Silicon carbide fibre reinforced glass-ceramic matrix composites have been investigated as a structural material for use in oxidizing environments to temperatures of 1000° C or greater. In particular, the composite system consisting of SiC yarn reinforced lithium aluminosilicate (LAS) glass-ceramic, containing ZrO₂ as the nucleation catalyst, has been found to be reproducibly fabricated into composites that exhibit exceptional mechanical and thermal properties to temperatures of approximately 1000° C. Bend strengths of over 700 MPa and fracture toughness values of greater than 17 MN m^–3/2 from room temperature to 1000° C have been achieved for unidirectionally reinforced composites of 50 vol% SiC fibre loading. High temperature creep rates of 10^–5 h^–1 at a temperature of 1000° C and stress of 350 MPa have been measured. The exceptional toughness of this ceramic composite material is evident in its impact strength, which, as measured by the notched Charpy method, has been found to be over 50 times greater than hot-pressed Si₃N₄.     

Mechanical and thermal properties of silicon-carbide composites fabricated with short Tyranno® Si-Zr-C-O fibre

Silicon carbide (SiC) composites reinforced with 10–50 mass% (10.5–51.2 vol%) of short Tyranno® Si-Zr-C-O fibre (average length 0.5 mm) and 0–10 mol% of Al₄C₃as a sintering aid were fabricated using the hot-pressing technique. Firstly, the effect of Si-Zr-C-O fibre addition on the relative density (bulk density/true density) of the SiC composite hot-pressed at 1800 °C for 30 min was examined by fixing the amount of Al₄C₃to be 5 mol%. Although the relative density was reduced to 87.4% for 10 mass% of Si-Zr-C-O addition, further increases in the amount of Si-Zr-C-O fibre increased density to a maximum of 92.8% at 40 mass% of fibre addition. Secondly, the effect of varying the amount of Al₄C₃addition on the relative density was examined by fixing the amount of Si-Zr-C-O fibre to be 40 mass%. The optimum amount of Al₄C₃addition for the fabrication of dense SiC composite was found to be 5 mol%. The fracture toughness of the hot-pressed SiC composites with 20–40 mass% of Si-Zr-C-O fibre addition (amount of Al₄C₃: 5 mol%) was 3.2–3.4 MPa · m^1/2and approximately 1.5 times higher than that (2.39 MPa · m^1/2) of the hot-pressed SiC composite with no Si-Zr-C-O fibre addition. SEM observation showed evidence of Si-Zr-C-O fibre debonding and pull-out at the fracture surfaces. The hot-pressed SiC composite with 5 mol% of Al₄C₃and 40 mass% of Si-Zr-C-O fibre additions showed excellent heat-resistance at 1300 °C in air due to the formation of a SiO₂layer at and near exposed surfaces.     

Microstructure and mechanical properties of B6O-B4C sintered composites prepared under high pressure

Sintered composites in the B₆O-xB₄C (x = 0–40 vol%) system were prepared under high pressure and high temperature conditions (3–5 GPa, 1500–1800°C) from the mixture of in-laboratory synthesized B₆O powder and commercially available B₄C powder. Relationship among the formed phases, microstructures and mechanical properties of the sintered composites was investigated as a function of sintering conditions and added B₄C content. Microhardness of the sintered composite was found to increase with treatment temperature up to 1800°C, while fracture toughness decreased slightly. Maximum microhardness of Hv 46 GPa was obtained from B₆O-30vol%B₄C sintered composite under the sintering conditions of 4 GPa, 1700°C and 20 min.