Self-Consistent Method to Calculate Fiber Interactions in a SiC/Al2O3 Ceramic Composite

The sintering of Al₂O₃/SiC ceramic composite leads to a state of high internal stresses in the composite material at room temperature because of the difference in thermal contraction between matrix and particles. It has been shown in a previous work¹ that the interaction among fibers must be accounted for in order to predict correctly the residual stresses. In the present paper we develop a numerical scheme that permits taking into account such interaction for an arbitrary distribution of fiber directions (DFD) and for completely anisotropic properties of the phases. We apply the formulation to calculate the average strain in the matrix (due to the interaction among fibers) and the effective thermal coefficients of the composite. We find that the average strain in the matrix depends strongly on the DFD and that the predictions agree with measurements done by Majumdar and Kupperman.³ We prove that the effective thermal coefficients of the composite are not sensitive to the DFD when the matrix and the fibers exhibit isotropic thermal and elastic properties. Finally, we analyze the effect of the DFD and of the fiber interaction on the internal stresses inside the SiC fibers and compare with experimental values.     

Effect of Inclusion Size on the Densification of ZnO–Zn7Sb2O12

Two-step densification curves, observed in the constant-rate heating of ZnO–Zn₇Sb₂O₁₂ composites, have been analyzed in correlation with the effect of inclusion particles (Zn₇Sb₂O₁₂). In the presence of these inclusion particles, the ZnO matrix is divided into two regions with different densification characteristics depending on the interaction with the particles. The linear shrinkage at the end of the first step depends on the inclusion size as well as on its volume fraction. The fractional volume of the region influenced by the inclusion particles has been estimated from the densification curve, and the size of the region influenced by an inclusion particle is found to increase with increasing inclusion size.     

Fracture Toughness of Al2O3 with an Unstabilized ZrO2Dispersed Phase

The fracture toughness of Al₂O₃ is considerably increased by the incorporation of fine monoclinic ZrO₂ particles. Hot-pressed composites containing 15 vol % ZrO₂ yield K_lcvalues of ∼ 10 MN/m^3/2, twice that of the A1₂O₃ matrix. It is hypothesized that this increase results from a high density of small matrix microcracks absorbing energy by slow propagation. The microcracks are formed by the expansion of ZrO₂during the tetragonal → monoclinic transformation. Since extremely high tensile stresses develop in the matrix, very small ZrO2 particles can act as crack formers, thus limiting the critical flaw size to small values.     

Tribological Properties of Polycrystalline Ti3SiC2 and Al2O3-Reinforced Ti3SiC2 Composites

Tribological properties of Ti₃SiC₂ and Al₂O₃-reinforced Ti₃SiC₂ composites (10 and 20 vol% Al₂O₃) were investigated by using an AISI-52100 bearing steel ball dryly sliding on a linear reciprocating athletic specimen. The friction coefficients were found varying only in a range of 0.1 under the applied loads (2.5, 5, and 10 N), and the wear rates of the composites decreased with increasing Al₂O₃ content. The enhanced wear resistance is mainly attributed to the hard Al₂O₃ particles nail the surrounding soft matrix and decentrale the shear stresses under the sliding ball to reduce the wear losses.     

Mechanical Properties of β-Si3N4-Whisker/Si3N4-Matrix Composites

Composites containing 30 vol%β-Si₃N₄ whiskers in a Si₃N₄ matrix were fabricated by hot-pressing. The composites exhibited fracture toughness values between 7.6 and 8.6 MPa · m^1/2, compared to 4.0 MPa · m^1/2 for unreinforced polycrystalline Si₃N₄. The improvements in fracture toughness were attributed to crack wake effects, i.e., whisker bridging and pullout mechanisms.     

Neutron Diffraction Measurements of the Residual Stresses in Al2O3-ZrO2 (CeO2) Ceramic Composites

High-resolution neutron powder diffraction was used to study the residual stresses in Al₂O₃-ZrO₂ (12 mol% CeO₂) ceramic composites containing 10, 20, and 40 vol% ZrO₂ (CeO₂). The diffraction data were analyzed using the Rietveld structure refinement technique. The analysis shows that for all samples, the CeO₂-stabilized tetragonal ZrO₂ particles are in tension and the Al₂O₃ matrix is in compression. For both the ZrO₂ particles and the Al₂O₃ matrix, the average lattice strains are anisotropic and increase approximately linearly with a decrease in the corresponding phase content. It is shown that these features can be qualitatively understood by taking into consideration the thermal expansion mismatch between the ZrO₂ and Al₂O₃ grains. Also, for all composite samples, the diffraction peaks are broader than the instrumental resolution, indicating that the strains in these samples are inhomogeneous. From an analysis of the refined peak shape parameters, the average root-meansquare strain, which describes the distribution of the inhomogeneous strain field, was determined. Finally, the average residual stresses were evaluated from the experimentally determined average lattice strains and compared with recent results of X-ray measurements on similar composites.     

Growth of Single-Crystal and Polycrystalline Thin Films of MgAl2O4 and MgFe2O4

Single-crystal and polycrystalline films of Mg-Al₂O₄ and MgFe₂O₄ were formed by two methods on cleavage surfaces of MgO single crystals. In one procedure, aluminum was deposited on MgO by vacuum evaporation. Subsequent heating in air at about 510°C formed a polycrystalline γ-Al₂O₈ film. Above 540°C, the γ-Al₂O, and MgO reacted to form a single-crystal MgAl₂O₄ film with {001} MgAl₂O₄‖{001} MgO. Above 590°C, an additional layer of MgAl₂O₄, which is polycrystalline, formed between the γ-Al₂O₃ and the single-crystal spinel. Polycrystalline Mg-Al₂O₄ formed only when diffusion of Mg²⁺ ions proceeded into the polycrystalline γ-Al₂O₃ region. Corresponding results were obtained for Mg-Fe₂O₄. MgAl₂O₄ films were also formed on cleaved MgO single-crystal substrates by direct evaporation, using an Al₂O₃ crucible as a source. Very slow deposition rates were used with source temperatures of ∼1350°C and substrate temperatures of ∼800°C. Departures from single-crystal character in the films may arise through temperature gradients in the substrate.     

Determination of Residual Surface Stresses Caused by Grinding in Polycrystalline Al2O3

Residual surface stresses introduced into polycrystalline Al₂O₃ during diamond grinding (320 grit) were examined by an X-ray direction technique commonly used for metals. Compressive stresses, estimated to be in the range 135 to 170 MPa and to extend 15 μm deep, were observed at the surface. It is believed that the compressive surface layer coincides with the plastic layer produced by the elastie/plastic interaction of the abrasive grains with the ceramic. The results are discussed with regard to the effect of the compressive layer on the extension of surface cracks.     

Microstructure and Short-Term Oxidation of Hot-Pressed Si3N4/ZrO2(+Y2O3) Ceramics

Composite ceramic materials based on Si₃N₄ and ZrO₂ stabilized by 3 mol% Y₂O₃ have been formed using aluminum isopropoxide as a precursor for the Al₂O₃ sintering aid. Densification was carred out by hot-pressing at temperatures in the range 1650° to 1800°C, and the resulting micro-structures were related to mechanical properties as well as to oxidation behavior at 1200°C. Densification at the higher temperatures resulted in a fibrous morphology of the Si₃N₄ matrix with consequent high room-temperature toughness and strength. Decomposition of the ZrO₂ grains below the oxidized surface during oxidation introduced radial stresses in the subscalar region, and from the oxidation experiments it is suggested that the ZrO₂ incorporated some N during densification.     

The Effect of Microstructure and Microcracking on the Thermal Conductivity of UO2-U4O9

Several microstructures were produced in dense polycrystalline UO₂-U₄O₉ specimens by cooling UO_2+x, solid solutions at different rates. Void formation (intragranular pores, grain-boundary microcracks) was observed in specimens which had a nonuniform distribution of the U₄O₉ precipitate; such formation was probably caused by the relief of stresses generated by differential thermal contraction. The microstructures were assessed quantitatively and used to calculate thermal conductivities from theoretical models. The effect of microcracking was calculated. Thermal conductivities were also determined from thermal diffusivity values measured by the laser-flash method. The thermal conductivity was primarily influenced by the amount of U₄O₉, present and the occurrence of voids, whereas the effect of U₄O₉, distribution was minor. Good agreement was obtained between theoretical predictions of thermal conductivity based on microstructure and experimental values.     

Novel Low-Temperature Processing Route of Dense Mullite Ceramics by Reaction Sintering of Amorphous SiO2-Coated γ-Al2O3 Particle Nanocomposites

Dense mullite ceramics were successfully produced at temperatures below 1300°C from amorphous SiO₂-coated gamma-Al₂O₃ particle nanocomposites (AS-gammaA). This method reduces processing temperatures by similar/congruent300°C or more with respect to amorphous SiO₂-coated alpha-Al₂O₃ particle microcomposites (AS-alphaA) and to other Al₂O₃-SiO₂ reaction couples. The good densification behavior and the relatively low mullite formation temperature make AS-gammaA nanocomposites an excellent matrix raw material for polycrystalline aluminosilicate fiber-reinforced mullite composites.     

Creep of Polycrystalline MgO-FeO-Fe2O3 Solid Solutions

Steady-state creep experiments were performed on hot-pressed polycrystalline MgO doped with Fe. Dead-load 4-point bend creep tests were conducted at stresses of 26 to 270 kg/cm², at temperatures of 1250° to 1450°C, in O₂ partial pressures of 1 to 10⁻⁹ atm, on specimens with grain sizes of 10 to 65 μm. Viscous steady-state creep was always observed when the grain size was stable. Experiments at variable P _O2's and temperatures were used to identify regimes of high (117 ± 10 kcal/mol) and low (81 ± 5 kcal/mol) activation energy. In the latter, creep rates were nearly independent of Fe dopant concentration and P _O2, whereas in the former creep rates were enhanced by increasing P _O2's and Fe dopant levels. The high- and low-activation-energy regimes were interpreted as diffusional creep controlled primarily by Mg lattice diffusion and O grain-boundary diffusion, respectively.     

High-Temperature Creep of Y2O3-Stabilized ZrO2

The compression creep behavior of Y₂O₃-stabilized ZrO₂ (YSZ) was studied at temperatures to 2000 ° C. The function of Y₂O₃ content and grain size was tested in specimens with various impurity concentrations and porosity distributions. For relatively fine-grained specimens, creep rates increased with the 1.5 power of the applied stress at low stresses and with the third power at high stresses. The results for coarse-grained specimens can, in general, be fit by the cube dependence. The 1.5 power can be reduced to a linear dependence by correcting for an apparent threshold stress, which decreases with increasing temperature. Creep activation energies for YSZ are 128 ± 10 kcal/mol, independent of Y₂O₃ content, impurity level, grain size, and porosity distribution. In addition, over a broad range of temperatures and stresses the absolute values of the steady-state creep rates are influenced only by grain size and O₂ partial pressure.     

Journal Effect of a Liquid Phase on the Sintering of Heterogeneous YBa2Cu3O6+x Compacts

Dense, polycrystalline YBa₂Cu₃O_6+x inclusions were incorporated into YBa₂Cu₃O_6+x: powder in order to investigate the effect of nondensifying inclusions on the sintering behavior of the matrix. The presence of these inclusions caused a significant reduction in the densification rate of the matrix, as well as some microstructural damage. However, when approximately 2.5 vol% of a liquid phase was present during sintering, there was some retardation of densification in the early stages, but this disappeared with time. Also, the final sintered microstructures were damage-free and essentially identical to those of samples containing no inclusions. Possible roles for the liquid phase in correcting this microstructural damage are briefly discussed.     

Creep of Polycrystalline MgO and MgO-Fe2O3 Solid Solutions at High Temperatures

Polycrystalline MgO and MgO-Fe₂O₃ solid solutions (0.10 to 8.08 wt% Fe₂O₃) were fabricated to almost theoretical density by vacuum hot-pressing. Specimens were creep-tested in air under four-point dead-load conditions between 1000° and 1400°C at stresses between 50 and 550 kg/cm². Steady-state creep was never achieved in the experiments, which sometimes lasted more than 50 h. The strain rate vs time ( t ) data were described by an equation of the form = c₁/(t+C₂)^p , which is consistent with the assumptions that creep occurs at least in part by a "viscous" mechanism and that grain growth occurs simultaneously. Doping MgO with Fe₂O₃ enhanced the viscous contributions to creep and inhibited the nonviscous ones. Creep rates in these specimens increased with increasing Fe₂O₃ additions. The occurrence of simultaneous grain growth during the high-temperature creep of magnesiowustite (i.e. MgO-Fe₂O₃ solid solutions) was used in establishing the strain rate vs grain size dependence. The results of this study are consistent with a transition between grain boundary and lattice diffusion mechanisms as the grain size increases (4 to 44 μan). The creep of polycrystalline MgO is a mixed process in that viscous and nonviscous (dislocation) contributions are present.     

Orientation Relationships of Reactively Grown Ba6Ti17O40 and Ba2TiSi2O8 on BaTiO3 (001) Determined by X-ray Diffractometry

Fresnoite grows at 700° and 800°C, and Ba₆Ti₇O₄₀ grows at 1200°C with definite orientations, which are determined by X-ray diffraction pole figure analysis. Partially textured fresnoite is formed at higher temperatures. The SiO₂ films react with the BaTiO₃ crystals, forming the phases Ba₂TiSi₂O₈ (fresnoite) and Ba₆Ti₁₇O₄₀. At 700° and 800°C, both phases grow with definite orientations, which are determined by X-ray diffraction pole figure analysis. Partially textured polycrystalline phases are formed at higher temperatures.     

Creation of Ferroelectric, Single-Crystal Architecture in Sm0.5La0.5BGeO5 Glass

Using a novel, selective heating by Nd:YAG laser, a single-crystal architecture is created in a model glass system, Sm_0.5La_0.5BGeO₅, which devitrifies congruently into a ferroelectric phase of the same composition as the parent glass. The Sm³⁺ ions in glass absorb the light and heat the matrix locally resulting in devitrification. Initially, a polycrystalline spot is formed. However, with optimum laser power, scanning speed, and the depth of focus, one of the grains acts as the seed for further growth as a single crystal. By programming the relative displacement of the glass with respect to laser spot, desired single ferroelectric crystal architecture is created. The optical functionalities (guiding of light and second harmonic generation) of the architectures are shown, which demonstrate the viability of this method for constructing active elements in optical integrated circuits. The single-crystal nature of the architecture is confirmed from the electron backscattered diffraction results.     

Single Crystals of Pb(Mg1/3Nb2/3)O3—35 mol% PbTiO3 from Polycrystalline Precursors

A potentially more cost-efficient method of growing single-crystal relaxor-based ferroelectric materials has been investigated. Seed single crystals of Pb(Mg_1/3Nb_2/3)O₃(PMN)—;35 mol% PbTiO₃(PT) were embedded within polycrystalline powders and annealed at temperatures from 900° to 1200°C. The boundary of the single crystal migrated through the polycrystal matrix under the influence of grain boundary curvature; growth distances of several millimeters were observed, verifying the feasibility of the approach. The grown single crystals exhibited macroscopic cubic growth morphologies with (100) faces. Strain levels as high as 0.68% under an electric field of 30 kV/cm were observed in initial measurements.     

Cation Self-Diffusion in Polycrystalline Y2O3 and Er2O3

A tracer sectioning technique was used to measure cation self-diffusion coefficients in fully dense polycrystalline Y_aO₃ and Er₂O_s under oxidizing conditions. The results are described by the relations for Y₂O₃ (1400° to 1670°C), and for Er₂O₃ (1400° to 1700°C). The greater activation energy for erbium diffusion in erbia may be partly attributable to a mass effect.     

Crystallization of MgO-Al2O3-SiO2-ZrO2 Glasses

The crystallization of MgO-Al₂O₃-SiO₂-ZrO₂ glasses at 1000°C was studied. Isothermal heat treatments of a cordierite-based glass (2MgO.2Al₂O₃.5SiO₂= Mg₂Al₄Si₅O₁₈) with 7 wt% ZrO₂ produced surface crystallization of α-cordierite and tetragonal ZrO₂ ( t -ZrO₂). These phases advanced into the glass by cocrystallization of t -ZrO₂ rods in an α-cordierite matrix with a well-defined orientation relation. The t -ZrO₂ rods were unstable with respect to diffusional breakup (a Rayleigh instability) and decomposed into rows of aligned ellipsoidal and spheroidal particles. The t -ZrO₂ was very resistant to transformation to monoclinic symmetry. With a similar glass containing 15 wt% ZrO₂, surface crystallization of α-cordierite and t -ZrO₂ was accompanied by internal crystallization of t -ZrO₂ dendrites. Transformation of the dendrites to mono-clinic symmetry was observed under some conditions.