High-Temperature Creep Behavior of Polycrystalline SrZrO3

The high-temperature creep behavior of sintered polycrystalline SrZrO₃ containing 1.35 wt% Fe₂O₃ was investigated as a function of temperature, stress, grain size, and strain level over the ranges 1160° to 1275°C, 780 to 3110 psi, 0.45 to 2.04 μm, and 0.0014 to 0.014, respectively. A constant-load 4-point (pure bending) method was used to load the specimens. The creep rate is time-dependent, decreasing exponentially with strain, i.e.     , where the decay constant (β=118, measured at the 1560 psi stress level over the strain range 0.0014 to 0.014) is independent of temperature and grain size. No significant grain growth occurred during creep. The activation energy of 169±10 kcal/mol obtained for creep is relatively independent of temperature, stress, grain size, and strain level over the ranges investigated. The creep rate is directly proportional to the cube of the stress and the reciprocal of the grain size; this result is consistent with nonviscous creep theories based on dislocation generation and climb as the rate-controlling deformation mechanism.     

Creep of Dense, Polycrystalline Magnesium Oxide

Creep of polycrystalline MgO was studied using four-point transverse bending at 1380° to 1800°K and stresses from 1000 to 5000 psi. The effects of temperature, stress, and grain size on the creep rate were determined for grain sizes from 2 to 20μ. Activation energies for creep decreased sharply with increasing grain size from 96,000 cal/mole at 2μ to 54,100 cal/mole at 5.5μ and then remained constant over the grain-size range 5.5 to 20μ. Creep was attributed in part to a stress-directed diffusional mechanism controlled by extrinsic oxygen ion diffusion in the 5.5 to 20μ grain sizes, although the calculated ionic self-diffusion rates were higher than those predicted by the Nabarro-Herring theory. It is suggested that the discrepancy may be due to a vacancy formation mechanism, which is consistent with the observed formation of dislocation substructure and preferentially distributed porosity during creep, as well as with the observed decrease in creep rate with increasing creep strain.     

High-Temperature Creep Behavior of Mixed Conducting La0.5Sr0.5Fe1−xCoxO3-δ (0.5≤x≤1) Materials

Steady-state compressive creep rate of La_0.5Sr_0.5Fe_0.5Co_0.5O_3−δ (LSFC) and La_0.5Sr_0.5CoO_3−δ (LSC) is reported in the temperature region 900°–1050°C and stress range 5–28 MPa. The stress exponents for the two materials were 1.71±0.18 and 1.24±0.15, respectively. The activation energy for creep was considerably higher for LSC (619±56 kJ/mol) than for LSFC (392±28 kJ/mol). The grain size exponent for LSC was 1.28±0.14. Considerably higher creep rates were observed for both materials in N₂ compared with air. Relaxation by creep of chemical-induced stresses in oxygen-permeable membranes is addressed, especially at low partial pressure of oxygen.     

High Temperature Tensile Creep of Magnesium Oxide Single Crystals

The creep behavior and the dislocation substructure developed during creep were investigated for 〈011〉 oriented MgO single crystals creep tested in tension. Creep deformation was studied over stress and temperature ranges of 29.0 to 86.2 MN/m² and 1200 to 1500°C, and the minimum creep rate, ε, was found to obey the relation:

where σ = applied tensile stress, k = the Boltzmann constant, T = absolute temperature, n = 3.8 to 4.5, and A = ll × 10⁻² (MN/m²)^-4 s^-1. Dislocation substructures developed during creep were studied by transmission electron microscopy and etch pitting techniques. At 1400°C, the dislocation density, ρ , at 0.10 tensile creep strain depended on applied stress as ρασ ^2.1. Numerous dislocation loops and long straight dislocations were present, but subboundaries were seldom observed. The results are discussed in terms of two possible operative creep mechanisms: (1) a recovery process based on annealing out of dislocation dipoles and loops, and (2) dislocation glide limited by atmospheres of charged defects surrounding dislocations.     

Superplastic Deformation in Fine-Grained YBa2Cu3O7−x

The superplastic behavior of YBa₂Cu₃O_{7− x} ceramic superconductors was studied. Large compressive deformation over 100% strain was measured in the temperature range of 775°–875°C, with a strain rate of 1 × 10⁻⁵ to 1 × 10⁻³/s, and a grain size of 0.5–1.4 μm. The nature of the deformation was investigated in terms of three deformation parameters: the stress exponent ( n ), the grain size exponent ( p ), and the activation energy ( Q ). The measured values of these parameters were n = 2 ± 0.3, p = 2.7 ± 0.7, and Q = 745 ± 100 kJ/mol. With the aid of the deformation map, the deformation mechanism was identified as grain boundary sliding accommodated by grain boundary diffusion. The conclusion is consistent with the microstructural observations made by SEM and TEM: the invariance of equiaxed grain shape, the absence of significant dislocation activity, no grain boundary second phases, and no significant texture development.     

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.     

Deformation Behavior of Polycrystalline Aluminum Oxide

The steady-state creep behavior of polycrystalline aluminum oxide from 97 to 100% dense has been examined at temperatures from 1600° to 1800°C over a range of stresses from 100 to 2000 psi under four-point transverse bending. Grain size is shown to have an important effect on the deformation behavior. Stress-strain rate dependence for the fine-grained aluminum oxide (3 to 13μ) is of viscous behavior (°_ε∼σ). The strain rate is also inversely proportional to the square of the grain size (°_ε∼ 1/(GS)²). The creep behavior can be described by the Nabarro-Herring diffusional flow model although the diffusion coefficient does not agree with that for oxygen diffusion in sapphire. When the grain size becomes coarse, the Nabarro-Herring model no longer applies. Coarse-grained aluminum oxide (50 to 100μl) behaves plastically when deformed (°_ε∼σ). The strain rates observed on coarsegrained aluminum oxide are higher than one would predict from the deformation behavior of fine-grained aluminum oxide. This plastic flow probably occurs through some dislocation movement or glide mechanism.     

Creep Behavior and Grain-Boundary Sliding in Polycrystalline A12O3

The creep properties of polycrystalline A1₂O₃ (grain size 14 to 65 μm) were examined under compressive stresses of between 4,000 and 18,000 psi (27.6 and 124 MPa) in the range 1600° to 1700°C. Two distinct types of behavior were observed. The creep rate of medium-grained specimens (14 to 30 μm) could be described by ασ^1.2 / d² where σ is the applied stress and d is the grain size. These results are consistent with the Nabarro-Herring creep mechanism. For the coarse-grained (65 μm) specimens, the creep rate was related to the stress by ασ^2.6. This behavior was not related to cracking; instead, a dislocation mechanism was thought to be rate-controlling. Considerable evidence for grain-boundary sliding was seen, and measurements showed that grain-boundary sliding contributed between 46 and 77% of the total strain in the 3 medium-grained specimens examined and between 38 and 50% in the 3 coarsegrained specimens examined.     

Grain-Size Effect on Compressive Creep of Silicon-Carbide-Whisker-Reinforced Aluminum Oxide

The steady-state compressive creep of Al₂O₃ with 10 vol% SiC whiskers having grain sizes of 1.2, 2.3, and 4.0 μm has been measured at 1400°C in argon. The creep rate is related to the free volume within the whisker network, not the nominal grain size. The results are consistent with diffusional-controlled creep with different contributions from grain-boundary sliding. Under low stresses, only Liftshitz sliding is possible and the diffusional process controls deformation, while at stresses over a threshold, Rachinger sliding is the mechanism controlling deformation. The evolution between Liftshitz and Rachinger sliding is marked by a significant increase in the value of the stress exponent.     

High-Temperature Creep and Kinetic Demixing in (Co,Mg)O

The creep behavior of fine-grained (Co_0.5Mg_0.5)O and (Co_0.25Mg_0.75)O has been characterized as part of an investigation of kinetic demixing in solid-solution oxides due to a nonhydrostatic stress. (i) For low stresses and small grain sizes, the dominant deformation mechanism for both compositions is diffusional creep limited by the transport of oxygen along grain boundaries. The oxygen grain-boundary diffusivity, D _o ^b is independent of oxygen partial pressure. The values of ω D _o ^b , where ω is the grain-boundary width, that have been determined from the steady-state diffusional creep rates are given by ω D _o ^b =4.7×10⁻⁸ exp[-230 (kJ/mol)/ RT ] (cm³/s) for (Co_0.5Mg_0.5)O in the range 950° to 1200°C and ω D _o ^b =7.4 × 10⁻⁸ exp[-263 (kJ/mol)/ RT ] (cm³/s) for (Co_0.25Mg_0.75)O in the range 1100° to 1250°C. Since oxygen diffusion controls the rate of diffusional creep, kinetic demixing is not observed in deformed samples of either composition. (ii) For high stresses and large grain sizes, the dominant deformation mechanism in both cases is dislocation-climb-controlled creep, where the rate of dislocation climb is controlled by oxygen lattice diffusion. Based on the positive dependence of creep rate on oxygen partial pressure, it is concluded that oxygen diffuses through the lattice by an interstitial mechanism.     

High-Temperature Creep and Dislocation Etch Pits in Polycrystalline Beryllium Oxide

Compressive creep of high-density polycrystalline beryllium oxide was investigated in the range 1850° to 2050°C. Creep rate was dependent on the applied stress to the 2.5 power, and the apparent activation energy for creep was 145 kcal/mole. Etch pit studies showed that the dislocation density in tested specimens was two orders of magnitude greater than that in assintered material. The diffusion process controlling creep was ascribed to volume diffusion of the anion. The deformation behavior was governed by dislocation motion.     

Flexural Creep of an in Situ-Toughened Silicon Carbide

Flexural creep behavior is reported for an in situ -toughened SiC between 1100° and 1500°C in four-point bending. The flexural creep rate of this SiC, sintered with aluminum, boron, and carbon (ABC-SiC), exhibits linear stress dependence, low apparent activation energy, and low incidence of cavitation and dislocation production. Most grain boundaries in this ceramic contain 1–5 nm intergranular films. The creep rate is consistent with a grain-boundary transport mechanism involving diffusion along the grain-boundary film-SiC interfaces. The microstructure and grain boundaries have been examined using transmission electron microscopy to assess possible changes during creep, particularly in relation to the applied stress direction.     

Compressive Creep of SiC-Whisker-Reinforced Al2O3

Compressive creep of SiC-whisker-reinforced Al₂O₃ composites (0, 5, 15, and 25 wt% SiC) was measured in the temperature range of 1300° to 1500°C in air and argon. The creep resistance increased with increasing whisker concentration. The results indicated that the whiskers degraded in air, increasing strain rates compared to those in argon. Stress exponents between 1.0 and 2.0 and an activation energy of 620 ± 100 kJ/mol were measured. Transmission electron microscopy observations indicated that cavitation was minimal and that the deformed composites had the same dislocation structure as did the as-received samples.     

Creep Behavior of Potassium Chloride–Rubidium Chloride Solid Solution Alloys

The creep behavior of three KCl–RbCl solid solution alloys and pure KCl and pure RbCl single crystals compressed along the 〈100〉 direction was investigated at 600°C at stresses between 0.5 and 15 MPa. The reduced primary creep stage, a value of the stress exponent of about 3 for the KCl–20 mol% RbCl and KCl–30 mol% RbCl alloys versus about 5 for pure KCl and pure RbCl and the results of the stress reduction tests for these alloys are in good agreement with creep behavior observed in class I metallic solid solution alloys, where the creep rate is controlled by a dislocation glide process. The dislocation substructure developed in the KCl–RbCl alloys consisted of well-developed subgrains.     

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.     

Enhanced Creep Resistant Silicon-Nitride-Based Nanocomposite

Silicon nitride–silicon carbide nanocomposite has been prepared by an in situ method that utilizes C+SiO₂ carbo-thermal reduction during the sintering process. The developed material is nearly defect free and consists of a silicon nitride matrix with an average grain size of approximately 200 nm with inter- and intra-granular SiC particles with sizes of approximately 150 and 40 nm, respectively. The creep behavior was investigated in bending at temperatures from 1200° to 1450°C, under stresses ranking from 50 to 150 MPa in air. The stress exponents are in the interval from 0.8 to 1.28 and the apparent activation energy is 480 kJ/mol. A significantly enhanced creep resistance was achieved by the incorporation of SiC nanoparticles into the matrix. This is because of a change of the microstructure and grain boundary chemistry leading to a change of creep mechanism and creep rate.     

Experimental Assessment of Plasticity of Nanocrystalline 1.7 mol% Yttria Tetragonal Zirconia Polycrystals

High temperature mechanical behavior of nanocrystalline 1.7 mol% (3 wt%) yttria tetragonal zirconia polycrystals (nc-YTZP) was characterized by compression creep tests. The hot isostatically pressed nc-YTZP with mean grain size of 120 nm was subjected to grain growth to obtain grain sizes in the range of 120–310 nm. Direct measurements of the creep parameters were performed in the temperature range 1150°–1300°C and stress range 5–400 MPa. The strain rates at 1150°C ranged between 2 × 10⁻⁷ and 9 × 10⁻⁵ s⁻¹ when increasing the stress from 15 to 400 MPa. Values of the stress exponent, n =2.0±0.3, and the activation energy, Q =630±40 kJ/mol, were obtained for all test conditions. A value of the grain size exponent, p =1.5±0.3, was obtained at 1150°C in the stress range studied. Detailed microstructural observations revealed the absence of glassy phase at the grain boundaries. The creep parameters were compared with those from the literature, and the results were discussed in terms of the model recently developed by the authors, with a reasonable agreement.     

Deformation Mechanism of Fine-Grained Magnesium Aluminate Spinel Prepared Using an Alkoxide Precursor

Polycrystalline MgAl₂O₄ spinel with high purity and stoichiometric composition was prepared using alkoxide precursors. The average grain size of the polycrystal was fine (1.7 μm). The deformation mechanism of the polycrystal was investigated in air at temperatures of 1300°–1400°C. At 1300°C, oxygen lattice diffusion controlled the deformation, despite the fine grain size; however, increases in the temperature and applied stress caused cavities to nucleate and grow. Spinel possessed better creep resistance than alumina of comparative grain size. The effective diffusion coefficient was determined as follows: [formula omitted]     

Comparison of Tensile and Compressive Creep Behavior in Silicon Nitride

The creep behavior of a commercial grade of Si₃N₄ was studied at 1350° and 1400°C. Stresses ranged from 10 to 200 MPa in tension and from 30 to 300 MPa in compression. In tension, the creep rate increased linearly with stress at low stresses and exponentially at high stresses. By contrast, the creep rate in compression increased linearly with stress over the entire stress range. Although compressive and tensile data exhibited an Arrhenius dependence on temperature, the activation energies for creep in tension, 715.3 ± 22.9 kJ/mol, and compression, 489.2 ± 62.0 kJ/mol, were not the same. These differences in creep behavior suggests that mechanisms of creep in tension and compression are different. Creep in tension is controlled by the formation of cavities. The cavity volume fraction increased linearly with increased tensile creep strain with a slope of unity. A cavitation model of creep, developed for materials that contain a triple-junction network of second phase, rationalizes the observed creep behavior at high and low stresses. In compression, cavitation plays a less important role in the creep process. The volume fraction of cavities in compression was ∼18% of that in tension at 1.8% axial strain and approached zero at strains <1%. The linear dependence of creep rate on applied stress is consistent with a model for compressive creep involving solution–precipitation of Si₃N₄. Although the tensile and compressive creep rates overlapped at the lowest stresses, cavity volume fraction measurements showed that solution–precipitation creep of Si₃N₄ did not contribute substantially to the tensile creep rate. Instead, cavitation creep dominated at high and low stresses.     

Harper–Dorn and Power-Law Creep in Single-Crystalline Magnesium Oxide

The creep behavior of single-crystalline MgO tested in the 〈100〉 direction is reviewed in the temperature range 1300° to 1800°C. At low stresses, the stress exponent is equal to about unity, and the deformation process is attributed to Harper–Dorn creep. At high stresses, the stress exponent is equal to approximately 5 and the deformation process is attributed to dislocation glide controlled by climb. The creep behavior in both regions is successfully predicted by an internal stress model for Harper–Dorn creep.