Mullite–Aluminum Phosphate Laminated Composite Fabricated by Tape Casting

Mullite–aluminum phosphate (3Al₂O₃·2SiO₂/AlPO₄) laminated composites were fabricated by tape casting. AlPO₄ had a density of 1.56 g/cm³, which corresponds to 61% of theoretical density, and a bending strength of 1.5 MPa after sintering at 1600°C for 10 h. The aluminum phosphate functioned as a porous, weak, and chemically stable interphase which was able to deflect cracks in a laminated composite. To increase the strength of the weak interphase material, 10 and 30 vol% of mullite were added.     

Microstructure and Mechanical Properties of Mullite–Silicon Carbide Composites

Mullite-SiC-whisker composites were prepared by powder processing using two commercial SiC whiskers. These composites were prepared by sintering rather than hot-pressing. A mulliteSlC-powder composite and a base line mallite material were also prepared for comparison with the two whisker composite materials. Fracture toughness measurements showed significant enhancement in only one of the whisker composite materials. The microstructure of the four materials was examined by scanning electron microscopy and transmission electron microscopy to assist in the explanation of the mechanical behavior of these composites. The examinations suggested that most of the toughening results from second-phase particles, with only limited toughening from effects associated with whiskers per se. In one case, higher toughness was partially associated with the formation of sialon phase by reaction with the whiskers and the furnace environment.     

Mullite/Alumina Particulate Composites by Infiltration Processing

A method has been developed for incorporating mullite into alumina by infiltrating an alumina preform with a prehydrolyzed ethyl silicate solution, followed by heating to decompose the infiltrant, form mullite, and densify the mullite/alumina composite. It has been found that the major portion of the weight loss of gelled ethyl silicate sols occurs in the 250° to 350°C range. Mullite formed in infiltrated bodies at ∼1475°C and specimens containing 12 to 15 vol% mullite reached 98.5% of the theoretical density after heating for 2 h at 1650°C. The mullite was found to be well dispersed within the alumina matrix and its presence decreased grain growth in the alumina by more than an order of magnitude.     

Alumina Agglomerate Effects on Toughness-Curve Behavior of Alumina–Mullite Composites

Toughness-curve ( T -curve) behavior of composites of spherical, polycrystalline, coarse-grained, alumina agglomerates dispersed throughout a constant-toughness, fine-grained, 50–50 vol% alumina–mullite matrix has been evaluated as a function of agglomerate content for the range 15 to 45 vol%. T -curve behavior was evaluated using the indentation-strength method. Increasing alumina agglomerate content resulted in a progressive increase of large indentation load strengths with negligible change of plateau strength levels at small indentation loads. This behavior is consistent with underlying T -curves that rise to greater values and are shifted toward longer crack lengths with increasing agglomerate content, suggesting that both bridge spacing and bridge potency increase with increasing agglomerate content over the range tested. The proposed relationships between bridge spacing and agglomerate content, and bridge potency and agglomerate content, are rationalized in terms of residual stress considerations. The indentation-strength data also demonstrated that the composite containing the greatest alumina agglomerate content, 45 vol%, exhibited the greatest flaw tolerance.     

Influence of the Metal Particle Size on the Crack Growth Resistance in Mullite–Molybdenum Composites

The R -curve for mullite–molybdenum (32 vol%) composites, which were obtained at 1650°C under reducing conditions with three different Mo average grain sizes (1.5, 3, and 9 μm), was estimated by the indentation-strength method and compared with that monolithic mullite obtained under similar conditions. The composites material exhibited rising R -curve behavior. The composite with larger grain size, however, displayed better damage tolerance and higher resistance to crack growth. Microscopic observation of the crack path revealed, in the composites, the systematic presence of dispersoids acting as bridging sites in the crack wake. Therefore, the increased fracture toughness of these ceramic-matrix composites with adherent ductile phase can be attributed to clamping forces applied by metal ligaments that bridge the crack faces behind the crack front. These clamping forces retard the crack from opening as an external stress is applied. It was inferred that this superior performance of the larger Mo particle size composite can be attributed mainly to more effective bridging of the metal grains. Because of this, a higher applied stress intensity will be required to propagate the crack tip. These results suggest that the rising R -curve should be proportional to the metal grain size, since the grain bridging area is proportional to the metal grain size.     

莫来石—钛酸铝复相陶瓷的高温强度与热分解

本文介绍了莫来石－钛酸铝复相陶瓷的制备工艺及其主要性能，重点对它的高温强度、热分解及抗热震性等进行了讨论并提出了我们的见解。     

Effect of Yttrium Aluminum Garnet Additions on Alumina-Fiber-Reinforced Porous-Alumina-Matrix Composites

The effects of incorporating yttrium aluminum garnet (YAG) into a porous alumina matrix reinforced with Nextel 610 alumina fibers were investigated. Composites with various amounts of YAG added to the matrix were prepared to determine its effect on retained tensile strengths after heating to 1100° and 1200°C. Strengths of YAG-containing composites were slightly lower than those of an all-alumina-matrix composite after heating for 5 h to 1100°C. However, after heating for 5 or 100 h at 1200°C, all the YAG-containing composites displayed greater strengths and greater strains to failure than the all-alumina composite. At the higher temperature, the presence of YAG is believed to inhibit the densification of the matrix, which helps to maintain higher levels of porosity and weaker interparticle bonding that allows for crack-energy dissipation within the matrix. A reduction in grain growth of the fibers by the presence of segregated Y was also observed, which may also contribute to higher fiber strength, thereby increasing the retained strengths of the YAG-containing composites.     

Mullite—Alumina Composites by Extrusion

The rheological properties of a paste containing chopped alumina fiber and particulate silica suspended in a gelled boehmite liquid phase have been evaluated using a physically based extrusion model. When sintered, the paste formed a mullite-alumina fiber composite. Extrudates with fiber volumes up to 30% in the sintered product were prepared. During extrusion, the pressure drop was largely independent of extrudate velocity, fiber length, and the fiber concentration. All pastes showed significant yield behavior leading to good postextrusion shape retention. For any given fiber length, it was shown that there exists a critical volume fraction above which fiber-fiber interactions are so great that both yield and wall shear stresses increase. At these high concentrations of fiber, inhomogeneities also increase. Up to the critical volume fraction, dispersed wet fibers produced lower extrusion parameters than when dry fibers were used as the starting material. The observed behavior is explained in terms of low viscosity liquid formation above the yield point of the boehmite gel.     

Microstructure and Composition of Alumina/Aluminum Composites Made by Directed Oxidation of Aluminum

Two Al₂O₃/Al composites, grown by the directed oxidation of molten Al alloys at 1400 and 1600 K, were investigated by X-ray diffraction, optical microscopy, scanning electron microscopy, transmission electron microscopy, and wet chemical analysis. The materials were found to contain a continuous network of Al₂O₃, which was predominantly free of grain-boundary phases and was made up of nanometer- to micrometer-sized crystallites, a continuous network of Al alloy, and isolated inclusions of Al alloy. No crystallographic orientation was observed in the metallic phase, whereas the Al₂O₃ was oriented with its c axis parallel to the growth direction. The higher process temperature yielded a lower metal content and less connectivity of the metallic consituent.     

Mullite Alumina Particulate Composites by Infiltration Processing: II, Infiltration and Characterization

Mullite/alumina composites were fabricated by infiltrating porous alumina preforms with a hydrolyzed ethyl silicate sol. Evidence is presented which suggests that initial infiltration occurred without complete filling of the porosity by the sol. Multiple infiltrations were used to increase the amount of SiO₂ introduced but led to blockage of the pores in the surface of the preform. Sintered bodies had concentration gradients, SiO₂ decreasing from the surface inward. Although mullite limited grain growth in alumina, in partially modified bodies large grains (>1 mm) with a preferred orientation were observed at the interface between the two zones.     

Synthesis of Thermally Stable χ-Alumina by Thermal Decomposition of Aluminum Isopropoxide in Toluene

Thermal decomposition of aluminum isopropoxide in toluene at 315°C resulted in χ-alumina that had high thermal stability, whereas the reaction at lower temperatures resulted in formation of an amorphous product. The χ-alumina thus obtained directly transformed to α-alumina at ∼1150°C, bypassing the other transition alumina phases, whereas the amorphous product transformed to γ-alumina and then to θ-alumina before final transformation to α-alumina. When the χ-alumina, solvothermally synthesized at 315°C, was recovered by the removal of the solvent at the reaction temperature, thermal stability of the product was improved further. This procedure is convenient because it avoids bothersome work-up processes that yield large-surface-area and large-pore-volume alumina.     

Mullite/Alumina Particulate Composites by Infiltration Processing: III, Mechanical Properties

The effect of incorporating mullite into alumina by an infiltration process on the mechanical properties was investigated. Data for Young's modulus, strength, and fracture toughness for various composite compositions were compared with those for the unreinforced matrix (alumina). Measurements of Young's modulus by a resonance technique showed that the addition of mullite decreased Young's modulus. Up to 14 vol%, these changes were close to those expected, but above this mullite content, the decrease was more dramatic and indicated specimen damage during processing. The addition of mullite led, in some cases, to increases of more than 60% in both the strength (biaxial flexure) and indentation fracture toughness. These increases have been attributed to the method of introducing mullite and the resulting residual compressive surface stresses. The strength of the indented composite bodies deviated from the ideal behavior, indicating the probability of R -curve behavior in these materials.     

Residual Stress in Alumina–Mullite Composites

Lattice strains have been measured by neutron diffraction from the alumina matrix in alumina–mullite composite cylinders. Infiltration processing results in a macroscopic variation of mullite concentration and residual stress throughout the samples. At the midheight of the cylinder, the stress component parallel to the cylinder axis is in a compression of −130 ± 30 MPa with respect to the value near the top surface. At the surfaces, the stress component parallel to the surface is in a compression of −130 ± 30 MPa with respect to values near the midheight of the cylinder. An overall tensile shift of the macroscopic stress profile in a fully infiltrated specimen is interpreted as a grain interaction effect between the alumina and mullite constituents. The positional dependence of the mullite phase concentration is also determined by neutron diffraction.     

Mullite/Alumina Particulate Composites by Infiltration Processing: IV, Residual Stress Profiles

Residual stress profiles through mullite/alumina bodies prepared by an infiltration process were determined. In one approach, residual stress profiles were predicted by obtaining concentration profiles and treating the bodies as laminates. In a second approach, a strain gage technique in which part of the sample was ground away while recording the resulting strain was used. The results showed that residual compressive stresses existed in the surface region of all composite samples. The strain gage approach indicated values of surface compression in the range of 176 to 291 MPa, which were higher than those predicted using the laminate approach. The results were compared with changes in the mechanical properties and found to be consistent with the increases in the strength and indentation fracture toughness which resulted when mullite was added to alumina by the infiltration technique.     

Phase Relations and Microstructural Development of Aluminum Nitride–Aluminum Nitride Polytypoid Composites in the Aluminum Nitride–Alumina–Yttria System

AlN–AlN polytypoid composite materials were prepared in situ using pressureless sintering of AlN–Al₂O₃ mixtures (3.7–16.6 mol% Al₂O₃) using Y₂O₃ (1.4–1.5 wt%) as a sintering additive. Materials fired at 1950°C consisted of elongated grains of AlN polytypoids embedded in equiaxed AlN grains. The Al₂O₃ content in the polytypoids varied systematically with the overall Al₂O₃ content, but equilibrium phase composition was not established because of slow nucleation rate and rapid grain growth of the polytypoid grains. The polytypoids, 24 H and 39 R , previously not reported, were identified using HRTEM. Solid solution of Y₂O₃ in the polytypoids was demonstrated, and Y₂O₃ was shown to influence the stability of the AlN polytypoids. The present phase observations were summarized in a phase diagram for a binary section in the ternary system AlN–Al₂O₃–Y₂O₃ parallel to the AlN–Al₂O₃ join. Fracture toughness estimated from indentation measurements gave no evidence for a strengthening mechanism due to the elongated polytypoids.     

Boron Nitride–Aluminum Nitride Ceramic Composites Fabricated by Transient Plastic Phase Processing

BN–AlN ceramic composites have been successfully fabricated by a novel process referred to as transient plastic phase processing (TPPP). The process used BN as both the reactant phase and the matrix and Al as the transient plastic phase. The products AlN and AlB₁₂ were regarded as the reinforcing phases. With the addition of Al powder in BN, both the mechanical and thermal properties were improved. Relatively high green density (2.03 g/cm³, 82.0% of theoretical density (TD)) and as-sintered density (2.18 g/cm³, 92.6%TD), high bending strength (106 MPa), and high thermal conductivity (72 W/(m·K)) were attained for one kind of BN–AlN composite. A low thermal expansion coefficient of 2.0 × 10⁻⁶/K was also achieved.     

Mullite (3Al2O3·2SiO2)–Aluminum Phosphate (AlPO4), Oxide, Fibrous Monolithic Composites

Mullite–AlPO₄ fibrous monolithic composites were fabricated by a co-extrusion technique using ethylene vinyl acetate (EVA) as a binder. Processing routes such as mixing formulation, extrusion sequence, binder removal cycle, pressing, and sintering procedures are described. An effort to make tougher composites was conducted by modifying the microstructures of the composites. Different kinds of monolithic composites were fabricated by changing the number of filaments, and the composition and thickness of interphase layers, and their microstructural and mechanical properties were characterized. To make the interphase more porous and to facilitate debonding and fiber pullout in the composite, graphite was added as a fugitive "space filler" into the interphase material and then removed. A fibrous monolithic composite with a sintered interphase thickness of 5–10 μm and an interphase composition of 50 vol% graphite and 50 vol% AlPO₄ had a three-point bend strength and a work of fracture of 129 ± 2 MPa and 0.86 ± 0.05 kJ/m², respectively. This corresponded to 42% of the strength but 162% of the work of fracture when compared with the values for a single-phase mullite. Two-layer, mixed 50% two-layer:50% three-layer, and three-layer fibrous monoliths were fabricated and their microstructural and mechanical properties were studied. The difference in the sintering behaviors of the two-layer and three-layer composites is described.     

Mullite–Boron Nitride Composite with High Strength and Low Elasticity

Mullite–boron nitride (BN) composite with high strength, low Young's modulus, and highly improved strain tolerance was prepared by reactive hot pressing (RHP) using aluminum borates (9Al₂O₃·2B₂O₃ and 2Al₂O₃·B₂O₃) and silicon nitride as starting materials. Compared with the monolithic mullite, the composite RHPed at 1800°C showed 1.64 times (540 MPa) the strength, 70% (153 GPa) the Young's modulus, and 2.34 times (3.53 × 10⁻³) the strain tolerance. Transmission electron microscopy observation revealed that the composite had an isotropic microstructure with a fine mullite matrix grain size of less than 1 μm and nanosized hexagonal BN (h-BN) platelets of about 200 nm in length and 60–80 nm in thickness. The high strength was suggested to be from the reduced matrix grain size and the small toughening effect by the h-BN platelets.     

Stabilization of Cubic Zirconia by Aluminum Nitride

Cubic ZrO₂ is stabilized at room temperature by the addition of AIN. The percentage of c-ZrO₂ in the mixture of c-ZrO₂ and m-ZrO₂ increases linearly with the addition of up to 20 mol% AIN and decreases thereafter. Stabilization becomes complete at 50 mol% AIN. The lattice spacing of the cubic phase gradually expands up to 20 mol% AIN. A displacement reaction ZrO₂+ AIN → ZrN+Al₂O₃ occurs above 20 mol% AIN and is completed at 50 mol% AIN.