Creep and densification during anisotropic sintering of glass powders

The isothermal sintering behaviour of a barium magnesium aluminosilicate glass powder at 930°C was investigated using a heating microscope. The cylindrical samples exhibited a variable shrinkage anisotropy during sintering. The shrinkage anisotropy ratio, defined as the ratio of the relative change of height and diameter, varied linearly between 0.3 and 0.98 with the relative volume shrinkage during densification. Shrinkage anisotropy caused creep deformation of the samples. The creep rate varied exponentially with the densification rate and the ratio of creep to densification rates, , decreased as densification proceeded. This is in disagreement with most previous studies, which show a constant value of during the densification. Overall, the study points out the relevance of variable shrinkage anisotropy and how it affects the densification behaviour of glass powders.     

Conservation of the elastic and flexural moduli of osteopenic femoral cortical bone in experimental inflammatory arthritis in the rabbit*

Experimental inflammatory arthritis (EIA) produced by carrageenan injection provokes a rapid bone remodeling state with cortical and cancellous bone loss. The objective of this study was to determine whether changes in cortical mechanical properties and/or geometry occur in long bones, either near or remote to the site of inflammation. EIA was induced in the right tibio-femoral joint of rabbits over 56 days. The right humerus and right femur from 15 normal and 25 arthritis group animals were excized. Semi-cylindrical specimens of the medial cortical shaft were subjected to non-destructive four-point bending tests. Transverse sections at the four contact sites of the loading jig were photographed and digitized to obtain average cross-sectional area (A) and moment of inertia (I). Moment of inertia and slope of the load/deflection curve permitted calculation of modulus of elasticity (E) for each specimen. Load/time curves were also used to calculate per cent stress remaining in relaxation experiments. Per cent stress remaining, E, A, I and \sqrt {{\text{I/A}}} (radius of gyration) were examined for differences by bone (humerus, femur) and by treatment (N,A) using two way ANOVA. The induction of inflammatory arthritis did not significantly alter the modulus of elasticity in either the femur or humerus; however, arthritis reduced the moment of inertia from . This was observed in the femur (near the arthritic joint), but not in the humerus (remote from arthritic joint). Analysis of area and ratio I/A demonstrated that this geometric effect of treatment was due to reduced area without gross cross-sectional shape changes. Per cent stress remaining in the femur (but not in the humerus) was higher in the arthritis specimens than in the normal specimens . Thus, in this arthritis model, the principal mechanical or geometric effect on cortical bone was reduction of the cross-sectional area and moment of inertia. The viscoelastic relaxation response of bone was also altered, perhaps due to loss of water or collagen degradation.     

Defect structure of acceptor-doped calcium titanate at elevated temperatures

The defect structure of acceptor (Al or Cr)-doped polycrystalline calcium titanate was investigated by measuring the oxygen partial pressure dependence (at 10° to 10–18 atm) of the electrical conductivity at 1000 and 1050° C. The observed electrical conductivity data were proportional to for the oxygen pressure range < 10^–10 atm and proportional to for the oxygen pressure range ( 10^–7 atm. The conductivity values were observed to increase with the acceptor concentration in the p-type region with the shift in the conductivity minima towards lower oxygen partial pressure. The absolute value of the electrical conductivity in the acceptor-doped samples were lower in the n-type region compared to the values in the undoped CaTiO₃. Aluminium and chromium were found to be equally effective in acting as acceptor impurities in CaTiO₃. The defect chemistry of CaTiO₃ is dominated by the added acceptor impurities for the entire oxygen partial pressure range used in this investigation.     

Determination of standard Gibbs energies of formation of ternary oxides in the system Co-Sb-O by solid electrolyte emf method

An isothermal section of the phase diagram of the system Co-Sb-O at 873 K was established by isothermal equilibration and XRD analyses of quenched samples. The following galvanic cells were designed to measure the Gibbs energies of formation of the three ternary oxides namely CoSb₂O₄, Co₇Sb₂O₁₂ and CoSb₂O₆ present in the system.

Electrical conductivity in non-stoichiometric titanium dioxide at elevated temperatures

The electrical conductivity of polycrystalline titanium dioxide prepared by a liquid mix technique was measured for the oxygen partial pressure range of 10° to 10^–19 atm and temperature range of 850 to 1050° C. The data were found to be proportional to the –1/6 power of oxygen partial pressure for the oxygen pressure range 10^–19 to 10^–15 atm, and proportional to for the oxygen pressure range >10^–15 atm. The region of linearity where the electrical conductivity varied as the –1/4 power of increased as the temperature was decreased. There was evidence of p-type behaviour for 10^{ - 2}$$ " align="middle" border="0"> atm in the temperature range 950 to 850° C, although the measured data were insufficient to assign a pressure dependence. Electrical conductivity minima in the log against log plot moved to lower as the temperature was decreased in the range 950 to 850° C. The measured oxygen pressure dependence of electrical conductivity in the lowest region supports the oxygen vacancy defect model. The observed data are consistent with the presence of very small amounts of acceptor impurities. A binding energy of 0.67 eV between the acceptor impurity and its compensating oxygen vacancy was also determined.     

Thermal expansion of molybdenum in the range 1500–2800 K by a transient interferometric technique

The linear thermal expansion of molybdenum has been measured in the temperature range 1500–2800 K by means of a transient (subsecond) interferometric technique. The molybdenum selected for these measurements was the Standard Reference Material SRM 781 (a high-temperature enthalpy and heat capacity standard). The results are expressed by the relation where T is in K and l ₀ is the specimen length at 20°C. The maximum error in the reported values of thermal expansion is estimated to be about 1% at 2000 K and not more than 2% at 2800 K.Paper presented at the Ninth Symposium on Thermophysical Properties, June 24–27, 1985, Boulder, Colorado, U.S.A.     

Non-linear response of internal friction to tensile strain rate and frequency during plastic deformation of high-purity aluminium

The internal friction of high-purity aluminium during the process of plastic deformation was measured by a middle torsion pendulum on a modified tensile testing machine. The effects of tensile strain rate, , in the range of 0.73×10^–6 to 50×10^–6s^–1, and frequency of internal friction measurement, f, in the range of 0.38 to 2.6 Hz were studied. The results showed a non-linear dependence of internal friction, Q ^–1, on and f ^–1 or on (=2 f). The interrelationship between internal friction during the process of plastic deformation and dislocation motion, and the effect of non-linearity on the dynamic behaviour of dislocations are discussed.     

The constant stress tensile creep behaviour of a superplastic zirconia-alumina composite

A detailed study was conducted to evaluate the constant stress tensile creep behaviour of a superplastic 3 mol% yttria-stabilized zirconia-20 wt% alumina composite. The comprehensive experimental results indicate that creep deformation may be expressed in the form exp(–585 000/8.3T), where is the steady-state creep rate, is the imposed stress, is the linear intercept grain size andT is the absolute temperature. Microstructural observations revealed that there is very little dislocation activity, or change in grain size or shape. A detailed analysis was conducted to evaluate the possible rate-controlling mechanisms in terms of the experimentally determined mechanical properties and the microstructural observations. Based on the maintenance of an equiaxed microstructure and the strong grain size and stress dependence, it is concluded that creep occurs by a grain-boundary sliding/grain rearrangement process.     

Grain growth behaviour of the Al-Cu eutectic alloy during superplastic deformation

Grain growth behaviour of the Al-Cu eutectic alloy was investigated as a function of strain (ε), strain rate and deformation temperature (T) over = 10⁻² s⁻¹ and T=400 to 540°C. The grain size increases with increase in strain and temperature. Upon deformation to a fixed strain, the grain growth is generally seen to be more at lower strain rates. The rates of overall grain growth and due to deformation alone , however, increase with increasing strain rate according to and , respectively. The increase in the grain growth rate with strain rate is attributed primarily to the shorter time involved at higher strain rate for reaching a fixed strain. The activation energy for grain growth under superplastic conditions is estimated to be 79 kJ mol⁻¹.     

Anisotropic flow and fracture in beryl [Be3Al2(SiO3)6]

Flow and fracture resulting from Vickers indentation testing on {0 0 0 1} and {10 0 } planar orientations have been examined. Flow characterized by indent shape differentiation was analysed to belong to the slip system with planes of the types { 10 0} and {11 0}. The ensuing fracture paths were resolved to propagate along {1 0 0} and {1 1 } cleavage planes whileK _c values obtained for them were 0.196 and 0.248 MPam^1/2, respectively.     

How the Surface Resistance Rs of Patterned High-Tc Superconducting Thin Film Is Affected by the Film''s Edge

This paper defines an effective microwave surface resistance for the nonuniform distribution of microwave surface resistance R _s in the strip of a microstrip. It is proved that is equivalent to the expression of R _s used in experiments, and that the is dominated by the edge part, i.e., the area of width ²/2t from the strip edge, where is the magnetic penetration depth and t is the film thickness. Under the assumption that where is the component of rf magnetic field along the film thickness and n is an integer, the ratio of the contributions of the edge part and the rest of the strip to is calculated by using an approximate analytical expression of the surface current density distribution J _s in the strip and calculated by the London equation. The effect of film's edge on R _s was studied using a microstrip resonator. It is found that the perfectness of the edge could affect the magnitude of the power dependence of R _s significantly, which agreed with our analysis.     

Electrical conduction of partially stabilized zirconia Zr0.94Ca0.06O1.94 as a function of temperature and oxygen partial pressure

Partially stabilized zirconia (PSZ), Zr_0.94Ca_0.06O_1.94was prepared by a hot kerosene drying method and a conventional oxide wet-mixing method. The total d.c. conductivities of these zirconia specimens were measured by the three-terminal technique as a function of temperature in the range 1088 to 1285 K and oxygen partial pressure in the range 1 to 10^–24 bar. The specimen prepared by the hot kerosene drying method showed near oxygen ion conduction with four times higher conductivity than the specimen prepared by the conventional mixing method at T=1088–1285 K and bar. The higher oxygen pressure conductivity tended approximately towards a to dependence, indicative of p-type conduction, whereas the lower oxygen pressure conductivity tended to be virtually independent of oxygen pressure, indicative of oxygenion conduction. The activation energy was found to be 130 kJ mol^–1 at T=1088–1285 K, bar (air) for pure electron-hole conduction and 153kJ mol^–1 at T=1088–1285 K for ionic conduction.     

The Smallest Correction of an Inconsistent System of Linear Inequalities

The problem of calculating a point x that satisfies a given system of linear inequalities, A x #x2265; b, arises in many applications. Yet often the system to be solved turns out to be inconsistent due to measurement errors in the data vector, b. In such a case it is useful to find the smallest perturbation of b that recovers feasibility. This motivates our interest in the least correction problem and its properties.Let A x #x2265; b be an inconsistent system of linear inequalities. Then it is always possible to find a correction vector y such that the modified system A x #x2265; b #x2212; y is solvable. The smallest correction vector of this type is obtained by solving the least correction problem Let denote the convex cone which consists of all the points for which the system A x #x2265; u is solvable. Let denote the polar cone of . It is shown that the least correction problem has a simple geometric interpretation which is based on the polar decomposition of into and . A further insight into the least correction concept is gained by exploring the duality relations that characterize such problems.     

Effect of non-stoichiometry on the sintering of doped TiO2

The sintering of TiO₂ has been studied with respect to oxygen partial pressure ( ) and doping content. From the microstructural evolution, it is obvious that a decrease of the oxygen pressure promotes the densification with a comparatively smaller grain growth than in air sintering. This fact has been related with the influence of defects on the sintering. Both effects of and tantalum doping have been studied. They are interpreted on the basis of a model involving interstitial titanium, electron holes, titanium vacancies and complexes associating titanium vacancies with tantalum substituted titanium. This latter complex is probable according to previous microscopic studies of defects in TiO_2–x and may be important in highly doped compounds. The formation of such associates reduces the mobile defect concentration, however a decrease of the favour their dissociation. The titanium vacancies which are thus released allow the titanium ions to migrate, a necessary condition for the sintering.     

Structural properties of nickel manganite Ni x Mn3−x O4 with 0.5 ⩽x ⩽ 1

Single-phase nickel manganite spinels, Ni _x Mn_3–x O₄, with 0.5 x 1, were prepared by a careful thermal processing of nickel-manganese coprecipitated oxalate precursors. Powder X-ray diffraction analysis of the spinel revealed the presence of cubic single spinel phase with parametera which decreases with nickel content. The lattice parameter variation can be explained in terms of the distribution of Ni²⁺ ions on the octahedral sites. Therefore, a fine analysis of data shows that some Ni²⁺ ions (forx>0.56) are located in tetrahedral sites. The percentage of nickel in A-sites increases with nickel content (x) following the relation % Ni²⁺ in A sites =P = – 82.1x ²+192.4x–81.5 and thus the general formula for cation distribution is

Rheological behaviour and microstructure of stir-casting zinc-aluminium alloys

The influence of processing variables on the rheological and microstructural behaviour of stir-cast (rheocast) ZA-27 alloy (Zn-27 wt % Al-2wt % Cu) has been investigated experimentally. A concentric cylinder viscometer with shear rate range up to 650 sec^–1 was used to measure the apparent viscosity of the slurries. During continuous cooling and at high shear rates (300–640 sec^–1), non-dendritical materials obey the power-law fluid model, i.e. where _a is the apparent viscosity and the shear rate. At lower shear rates (125 sec^–1), the slurries display dendritical-liquid mixture with viscosity up to 50 poises. Microstructural studies of continuously cooled materials reveal a clear tendency of primary particles to cluster. This phenomenon could be explained by the reduction of the amount of entrapped liquid in the particles.     

The effect of gas atmospheres on resistivity of indium tin oxide films at high temperature

The effects of heat treatment in Q₂, O₂ and N₂, and Ar gases on the high temperature (500 C) electrical resistivity of indium tin oxide (ITO) film 52 nm thick prepared by chemical spray pyrolysis method were studied. The partial oxygen pressure effect on the resistivity was found to be to . The resistivity changes for cyclic exchange of O₂ by Ar gas at 500 C. These lead to the conclusion that chemisorption of oxygen atoms in the film surface is dominant for this thin film, for thicker films such as 640 nm oxygen diffusion is found to occur. The Langmuir model of the monolayer isothermal adsorption of oxygen atoms in the surface is applicable to the rapid change of resistivity.     

Preparation of CuZr2P3O12 from alkoxide-derived gels: phase formation as a function of heat treatment

The phase formation in alkoxide gels with composition corresponding to CuZr₂P₃O₁₂ has been studied as a function of gel preparation and heat treatment. Two preparational methods have been examined. The chemicals used include Cu(NO)₃ · 3H₂O, Zr(n-OC₃H₇)₄ and either P₂O₅ or H₃PO₄, respectively. The P₂O₅ method results in the formation of di-phase gels. Heat treatment of these invariably gives multi-phase materials. Gels prepared by the H₃PO₄ method are completely amorphous and can be converted into porous glasses by heating to 500 °C. Calcination in the range 650 to 750 ° C results in the formation of a new CuZr₄P₆O₂₄ phase ( . Later, this prevents formation of mono-phase materials during heating to 1200 ° C. It is suggested that this behaviour is related to mixing of Cu²⁺ and Zr⁴⁺ in the normal copper and zirconium positions in the low-temperature -Nasicon. Calcination in the range 750 to 850 ° C results in the formation of the normal C2/c Cu²⁺-Nasicon which readily converts to mono-phase Cu⁺-Nasicon (CuZr₂P₃O₁₂) above 880 ° C. Only gels calcined in the range 750 to 850 ° C are useful for the fabrication of mono-phase CuZr₂P₃O₁₂ ceramics.     

Fracture toughness and fracture mechanisms of PBT/PC/IM blend

The static and impact fracture toughnesses of a polybutylene terephthalate/polycarbonate/impact modifier (PBT/PC/IM) blend were studied at different temperatures. The static fracture toughness of the blend was evaluated via the specific fracture work concept and the J-integral analysis. A comparison of these two analytical methods showed that the specific essential fracture work, W _e, was equivalent to the obtained by the ASTM E813-81 procedure, representing the crack initiation resistance of the material. The discrepancy between W _e and of ASTM E813-89 was caused by the extra energy component in consumed by a 0.2 mm crack growth. Impact fracture toughness was also analysed using the specific essential fracture work approach. When the fracture was elastic, W _e was equivalent to the critical potential energy release rate, G _IC, obtained via LEFM analysis. Temperature and strain-rate effects on the fracture toughness were also studied. The increase in impact toughness with temperature was attributed to two different toughening mechanisms, namely, the relaxation processes of the rubbery particles and the parent polymers in a relatively low-temperature range and thermal blunting of the crack tip at higher temperatures. The enhancement in static fracture toughness at temperatures below — 60 °C was thought to be caused by plastic crack-tip blunting, but the monotonic reduction in yield stress was largely responsible for the toughness decreasing with higher temperatures. The temperature-dependent fracture toughness data obtained in static tests could be horizontally shifted to match roughly the data for the impact tests, indicating the existence of a time-temperature equivalence relationship.     

Creep Behavior of Dispersion-Hardened Aluminum Materials

Dispersion-hardened aluminum materials of pure aluminum with extremely fine oxide and carbide dispersions and very fine grain sizes were creep-deformed under compressive loadings between 573 and 773 K. The creep behavior of the investigated materials is influenced by time, temperature, stress level and microstructure. An increasing content of dispersions causes increasing threshold stresses _thand resistances against creep. The Norton plots of the minimum creep rate versus stress are characterized by extremely high stress exponents n. On the basis of the threshold concept it is demonstrated that the same diffusion process dominates in the dispersion-hardened aluminum materials as in pure aluminum. Their true stress exponents n^*as the slopes of the best fit lines of the are close to 5. The threshold stress decreases considerably with increasing temperature due to the thermally activated recovery of long-range internal back stresses of quasi-planar dislocation structures on the grain boundaries.