The Measurement of Compressive Creep Deformation and Damage Mechanisms in a Single-Phase Alumina Part I Grain boundary sliding

Grain boundary sliding (GBS) has been hypothesized to act as the primary driving force for the nucleation and growth of grain boundary cavities in ceramics undergoing creep. In addition, GBS is often a major mode of deformation during high-temperature creep. This paper demonstrates the importance of GBS with mode II GBS measurements performed using a stereoimaging technique on a single-phase alumina tested under constant compressive stresses of 70 and 140 MPa at 1600 °C. Measurements were taken at constant time intervals during creep. The results support previous observations that GBS is stochastic and history independent. GBS displacements at given time intervals are shown to fit a Wiebull distribution. During steady-state creep, GBS displacements increased linearly with time at a constant sliding rate of 6.0 × 10–5 m s–1 at 70 MPa and 1.3 × 10–4 m s–1 at 140 MPa. Also, an average of 67% of the grain boundaries exhibited measurable sliding throughout the creep life of the 140 MPa test. Results of the GBS measurements are used to modify an existing creep model describing stochastic GBS. In part II of this paper [1], the GBS measurements reported are related to the associated creep cavitation measured in specimens tested under identical conditions.     

High-temperature deformation behaviour of YBa2Cu3O7−x

High-temperature compression tests were performed in air for YBa₂Cu₃O_7–x polycrystals with grain sizes of 3 and 7 m at various strain rates between 1.3×10^–5 and 4×10^–4s^–1 and at temperatures between 1136 and 1253 K. Steady state deformation appeared above 1203 K for both samples. A stress exponent of 1.3 and an activation energy of 150 kJ mol^–1 were evaluated. The compression tests and microstructural observations revealed that there was a difference in deformation mechanism above and below 1203 K. The dominant mechanism was diffusional creep associated with grain-boundary sliding above 1203 K, and dislocation glide accompanied with grain-boundary sliding below 1203 K. The growth of anisotropic grains and their preferred arrangement were enhanced by deformation.     

Mechanical behaviour,percolation and damage of materials with viscous solid grain boundaries

The mechanical behaviour, percolation and damage mechanism of a aluminium alloy with viscous solid grain boundaries (GBs) at 465 °C have been characterized in experiments performed in tension or compression in the strain rate range of 10^–5-10^–2s^–1. It was found that grain-boundary sliding (GBS) occurs as strain rates below 10^–4s^–1. It was shown that the viscous solid interphase migrates during the process of deformation. In the case of tension, it was squeezed out of GBs parallel with the tension axis into GBs perpendicular to the axis and vice versa in the case of compression. This local percolation is discussed in terms of the viscosity of the interphase, gradient of local stresses and percolation time. The viscosity of the solid interphase is estimated. It was also found that cavitation depends on the type of stress (tension or compression) and the strain rate. Cavity nucleation occurs at multiple points when GBS happens or along G B facets in the absence of GBS. Cavity growth takes place along GBs at high normal stresses and the cavity coalsescence leads to saw-tooth fracture.     

Grain-boundary de-segregation and intergranular cohesion in Si-Al-O-N ceramics

The influence of heat-treatment on high-temperature creep and sub-critical crack growth in hot-pressed Si-Al-O-N ceramics has been analyzed from microstructural evidence and determination of stress exponents and activation energies. The most significant change is the suppression of cavitation during creep and of the cavity-interlinkage mechanism for slow crack propagation. A creep mechanism of grain-boundary diffusion is characterized by stress exponent n=1 and unusually high activation energy >820 kJ mol^–1. The microstructural origin of the transformation in grain-boundary dominated properties is mainly the removal of triple-junction glassy residues within which cavities are nucleated. This is caused by grain-boundary diffusion of metallic impurities (Mg, Mn, Ca) into a surface silica oxidation layer, and consequent crystallization of the remaining glass components as . There is a continued improvement in grain-boundary cohesion and increased difficulty of grain-boundary diffusion following the stage at which triple-junction glass is removed. The resultant ceramics, in addition to superior mechanical behaviour, have an increased temperature for application due to a marked reduction in susceptibility to dissociation above 1400° C.     

Creep of austenitic 20% Cr/35% Ni stainless steels at low stresses

The present work comprises measurements of the secondary creep-rate at different stress levels with rates between about 2×10^–5 %/h and 10%/h and the grain-boundary sliding at 700° C in two austenitic 20 wt % Cr/35 wt % Ni stainless steels. One alloy was a pure 20 wt % Cr/35 wt % Ni steel, whereas the other contained about 0.5 wt % Ti and 0.5 wt % Al so that it precipitated during creep at 700° C. Special care was taken to assure equivalent microstructure in the specimens and precise creep conditions so as to obtain accurate and reproducible creep-rates. Both materials exhibited decreasing stress-dependence of the creep-rate at low stresses. Neither the stress-dependence of the creep-rate, nor the absolute creep-rate was consistent with diffusion-creep. The amount of grain-boundary sliding was measured separately by means of scribed grid lines on the creep specimens for the pure material at stresses above the creep yield. The values for the component of the creep-rate due to grain-boundary sliding coincide very well with the extrapolated line of the low-stress branch of the creep-rate/stress curve. All these results taken together suggest that the most likely explanation of the creep yield in 20 wt % Cr/35 wt % Ni steels is the one based upon grain-boundary sliding.     

Corrosion of silicon nitride ceramics under hydrothermal conditions

Corrosion behaviour of Si₃N₄ ceramics containing Y₂O₃, Al₂O₃ and AIN as sintering aids was investigated under hydrothermal conditions at 200–300 C and saturated vapour pressures of water for 1–10 days. Hydrothermal corrosion resulted in the dissolution of the Si₃N₄ matrix and the formation of a product layer consisting of the original grain-boundary phases and hydrated silica. The dissolution rate of Si₃N₄ ceramics decreased with decreasing crystallinity of the grain-boundary phase. The dissolution rate could be adequately described by a parabolic plot in the initial stage of the reaction. The apparent activation energies were 83.5–108 kJ mol^–1, and the bending strength of the corroded samples decreased from 600 to 400 MPa in the initial stage of the reaction upto a weight loss of 0.004 g cm^–2, and then was almost constant up to a weight loss of 0.012 g cm^–2.     

Creep behaviour of Si3N4/Y2O3/Al2O3/AIN alloys

The compression creep behaviour of pressureless sintered Y₂O₃/Al₂O₃/AIN-doped Si₃N₄ was studied between 1473 and 1673 K, under stresses ranging from 100–300 MPa. Strain rate versus stress and temperature analysis give a stress exponent n1 and an activation energy Q=860 kJ mol^–1. Microstructural change was investigated by transmission electron microscopy. The observed strain whorls, the stress exponent and the activation energy are indicative of a solution-diffusion-precipitation accommodated grain-boundary sliding where the diffusion through the glass is rate controlling.     

Effect of atmosphere on superplastic deformation behavior in nanocrystalline liquid-phase-sintered silicon carbide with Al2O3-Y2O3 additions

Nanocrystalline -SiC with additions of 5.135 wt% Al₂O₃ and 3.867 wt% Y₂O₃ was subjected to tensile deformation in order to study its microstructural behavior under the dynamic process. The liquid-phase-sintered body had a relative density of >95% and an average grain size of 190 nm. Tension tests were conducted at initial strain rates range from 3 × 10^–4 to 2 × 10^–5 s^–1, in the temperature range 1873–2048 K, in both argon and N₂ atmospheres. Although grain-boundary liquids formed by the additions vaporized concurrently with the decomposition of SiC and grain growth, the maximum tensile elongation of 60% was achieved in argon. The grain-boundary amorphous phase formed a crystalline phase during testing in an N₂ atmosphere and fracture occurred at <8% elongation. Grain-boundary sliding was still the dominant mechanism for deformation.     

Enhancement of the diffusional creep of polycrystalline Al2O3 by simultaneous doping with manganese and titanium

The effect of simultaneous doping with manganese and titanium on diffusional creep was studied in dense, polycrystalline alumina over a range of grain sizes (4–80m) and temperatures (1175–1250° C). At a total dopant concentration of 0.32–0.37 cation %, diffusional creep rates were enhanced considerably such that the temperature at which cation mass transport was significant was suppressed by at least 200° C compared to that observed in undoped material. The Mn-Ti (and Cu-Ti) dopant couple was far more effective in enhancing creep rates and suppressing sintering temperatures than the Fe-Ti couple. The enhanced mass transport kinetics are believed to be caused by significant increases in both aluminium lattice and grain-boundary diffusion. When aluminium grain-boundary diffusion is enhanced by increasing the concentration of divalent impurity (Mn²⁺, Fe²⁺) or by creep testing at low temperatures, creep deformation is Newtonian viscous.     

Effects of heat treatments on the creep properties of a hot pressed silicon nitride ceramic

Effects of heat treatment in an argon atmosphere at high temperatures for varying times on the creep properties of a Y₂O₃-Al₂O₃ (8-2 wt%) doped hot pressed silicon nitride (HPSN) ceramic were investigated. It was observed from the creep measurements that higher temperature, i.e. 1360C, and longer time, i.e. 8 h, heat treatment in an argon atmosphere improved the creep properties, (e.g. secondary creep rate) of this material. Heat treatment at a lower temperature of 1300C and for a shorter time of 4 h did not change the creep behaviour. Improvement of the creep properties was related to the crystallization of an amorphous grain boundary phase by heat treatment. Secondary creep rate parameters of the as-received material: stress exponent, n (2.95–3.08) and activation energy, Q (634–818 kJ mol^S–1), were in the range of values found by other investigators for various hot pressed silicon nitride ceramics.     

Zr-Hf interdiffusion in polycrystalline Y2O3-(Zr+Hf)O2

Lattice and grain-boundary interdiffusion coefficients were calculated from the concentration distributions determined for Zr-Hf interdiffusion in polycrystalline 16Y₂O₃·84(Zr_1–x Hf _x )O₂ withx=0.020 and 0.100. The lattice interdiffusion coefficients were described byD=0.031 exp [–391 (kJ mol^–1)/RT] cm² sec^–1 and the grain-boundary diffusion parameters byD=1.5×10^–6exp [–309(kJ mol^–1)/RT] cm³ sec^–1 in the temperature range 1584–2116° C. Comparison of the results with those for the systems CaO-(Zr+Hf)O₂ and MgO-(Zr+Hf)O₂ indicated that the Zr self-diffusion coefficient was insensitive to the dopants in the fluorite-cubic ZrO₂ solid solutions.     

Nonlinear electrical characteristics and dielectric properties of (Ca, Ta)-doped TiO2 ceramics

TiO₂ ceramics doped with 1.0 mol% Ca and different concentrations of Ta were obtained by sintering processing at 1450°C. The microstructures, nonlinear electrical behavior and dielectric properties of the ceramics were investigated. The samples have nonlinear coefficients of = 2.0–5.0 and ultrahigh relative dielectric constants which is up to 10⁵. Especially, the effects of Ta dopant on the nonlinear electrical characteristics and dielectric properties of the (Ca, Ta)-doped TiO₂ ceramics were studied in detail. When the concentration of Ta is 2.0 mol%, the sample exhibits the highest nonlinear coefficient and a comparatively lower dielectric constant. By analogy to a grain-boundary atomic defect model, the effects of Ta and the nonlinear electrical behavior of the TiO₂ system were explained.     

Superplastic deformation of the Pb-Sn eutectic

Dynamic observations of grain-boundary sliding during superplastic flow of the Pb-Sn eutectic are reported. These observations confirm the postulate that the dominant deformation mode during superplastic flow is grain-boundary sliding with localized deformation necessary to maintain grain coherency. Extensive grain-boundary sliding is also observed when the strain-rate and/or grain size is outside the superplastic flow regime. Stress relaxation tests were also carried out on the Pb-Sn eutectic. These tests provide data on the activation energy (45±5 kJ mol^–1), grain-size dependence (d ^–3), and stress dependence of superplastic flow in this alloy. A threshold stress of 1.3×10⁶N m^–2 for the onset of superplastic deformation is also observed.     

Creep in pure and two phase nickel-doped alumina

Creep in pure and two phase nickel-doped alumina has been investigated in the stress range 0.70 to 4.57 kgf mm^–2 (1000 to 6500 psi), and temperature range 1450 to 1800° C, for grain sizes from 15 to 45 m (pure alumina) and 15 to 30 um, (nickel-doped alumina). The effect of stress, grain size and temperature on the creep rate suggests that diffusion controlled grain-boundary sliding is the predominant creep mechanism at low stresses and small grain sizes. However, the stress exponents show that some non-viscous boundary sliding occurs even at the lowest stresses investigated. This mechanism is confirmed by metallographic evidence, which shows considerable boundary corrugation in the deformed aluminas. At higher stresses and larger grain sizes the localized propagation of microcracks leads to high stress exponents in the creep rate equation. The nickel dopant, which introduces an evenly distributed spinel second phase into the alumina matrix, increases the creep rate and enhances boundary sliding and localized crack propagation. The weakening effect of the second phase increases with grain size, and tertiary creep occurs at strains of 0.5% and below in large grained material.     

Transient creep behaviour of hot isostatically pressed silicon nitride

Transient creep is shown to dominate the high-temperature behaviour of a grade of hot isostatically pressed silicon nitride containing only 4 wt% Y₂O₃ as a sintering aid. Contributing factors to transient creep are discussed and it is concluded that the most likely cause of longterm transient creep in the present study is intergranular sliding and interlocking of silicon nitride grains. In early stages of creep, devitrification of the intergranular phase, and intergranular flow of that phase may also contribute to the transient creep process. The occurrence of transient creep precluded the determination of an activation energy on the as-received material. However, after creep in the temperature range 1330–1430°C for times exceeding approximately 1100 h, an apparent activation energy of 1260 kJ mol^–1 was measured. It is suggested that the apparent activation energy for creep is determined by the mobility and concentration of diffusing species in the intergranular glassy phase. The time-to-rupture was found to be a power function of the minimum strain rate, independent of applied stress or temperature. Hence, creep-rupture behaviour followed a Monkman-Grant relation. A strain rate exponent of – 1.12 was determined.     

Superplastic behaviour of YBa2Cu3O7−x /Ag superconductors

High-temperature deformation characteristics of YBa₂Cu₃O_7–x oxide (YBCO) and YBa₂Cu₃O_7–x /Ag composite (YBCO/Ag) in uniaxial compression have been investigated. A compression test was carried out at temperatures from 780–930°C at initial strain rates between 10^–6 and 10^–4 s^–1. YBCO/Ag composites with fine, dense and equiaxed grains were compressed over 120% with no indication of failure at higher temperatures, and the strain-rate sensitivity exponent, m, was found to be about 0.42–0.46 between 890 and 930°C. They are considered to be one indication of superplasticity. The activation energy for deformation was 500–580 KJ mol^–1. The specimens suffered grain growth slightly during the deformation at 930°C and the majority of growth might be a function of exposure time, temperature and silver content, but each grain maintained the equiaxed shape after extensive superplastic deformation. This is consistent with a grain-boundary sliding mechanism. The silver at grain boundaries acts to decrease the activation energy for deformation and promote the grain-boundary sliding.     

Tensile creep behaviour of a fibre-reinforced SiC-Si3N4 composite

The tensile creep behaviour of a SiC-fibre-Si₃N₄-matrix composite was investigated in air at 1350 C. The unidirectional composite, containing 30 vol % SCS-6 SiC fibres, was prepared by hot pressing at 1700 C. Creep testing was conducted at stress levels of 70, 110, 150 and 190 MPa. An apparent steady-state creep rate was observed at stress levels between 70 and 150 MPa; at 190 MPa, only tertiary creep was observed. For an applied stress of 70 MPa, the steady-state creep rate was approximately 2.5×10^–10 s^–1 with failure times in excess of 790 h. At 150 MPa, the steady-state creep rate increased to an average of 5.6×10^–8 s^–1 with failure times under 40 h. The creep rate of the composite is compared with published data for the steady-state creep rate of monolithic Si₃N₄.     

Grain growth in (Ca1−x,Mg x )Zr4(PO4)6 ceramics

Grain growth in (Ca_1–x ,Mg _x )Zr₄(PO₄)₆ (CMZP) ceramics in the final stage of sintering has been investigated. The grain growth in CMZP ceramics obeys the isothermal grain-growth kinetics with time exponent,n, lying between 1.8 and 2.4 which depends on magnesium content, indicative of a change in grain-growth rate. The time exponent for the grain growth of CMZP can be taken as 2.0 which implies that a normal grain growth develops in the CMZP ceramics. The apparent activation energy for grain growth demonstrates a maximum atx = 0.0 and a minimum atx = 0.1, with 103.2 and 39.4 kcal mol^–1, respectively, indicating that a small amount of magnesium promotes grain-boundary migration. The critical grain size for initiating microcracks in the CMZP increases with increasing magnesium and reaches 9–12 m whenx = 0.4.     

High temperature bending creep of a Sm-α-β Sialon composite

The four-point bending creep behavior of a Sm-- Sialon composite, in which Sm-melilite solid solution (denoted as M) was designed as intergranular phase, was investigated in the temperature range 1260–1350°C and stresses between 85 and 290 MPa. At temperatures less than 1300°C, the stress exponents were measured to be 1.2–1.5, and the creep activation energy was 708 kJ mol^–1, the dominant creep mechanism was identified as diffusion coupled with grain boundary sliding. At temperatures above 1300°C, the stress exponents were determined to be 2.3–2.4, and creep activation energy was 507 kJ mol ^–1, the dominant creep mechanism was suggested to be diffusion cavity growth at sliding grain boundaries. Creep test at 1350°C for pre-oxidation sample showed a pure diffusion mechanism, because of a stress exponent of 1. N^3– diffusing along grain boundaries was believed to be the rate controlling mechanism for diffusion creep. The oxidation and Sialon phase transformation were analyzed and their effect on creep was evaluated.     

Some observations of grain-boundary sliding in aluminium bicrystals tested at constant strain rate and constant rate of stress increase

Bicrystals of pure aluminium, aluminium/0.05 wt% and aluminium/0.30 wt% copper have been deformed in shear within the temperature range 350 to 600°C at a constant rate of grip displacement (300 m/h) and constant rates of increase of grain-boundary shear stress (0.30 to 1.04 g/mm^–2 min^–1). The stress/time, sliding/time and sliding/stress curves for these tests are presented together with metallographic observations. The stress/time curves exhibited changes in the strain-hardening rates which were accompanied by the occurrence of extensive crystal deformation. In many cases, following the change in strain-hardening rate and onset of extensive crystal slip, the extent of grain-boundary sliding was proportional to the shear stress on the boundary. The ratio of the extent of sliding to the grain-boundary shear stress increased with increasing test temperature. The temperature-dependence of the sliding behaviour, as reflected by the sliding/stress results, yielded apparent activation energies of 31 Kcal/mole in the temperature range 600 to 475°C and 8 Kcal/mole in the range 475 to 350°C.