Compressive Creep of Al2O3 Single Crystals

Aluminum oxide single crystals deformed by dislocation glide and deformation twinning during compressive creep at 1400° to 1700°C. The activation energy for basal slip was a function of the applied stress and agreed with activation energies previously measured by observation of yielding phenomena. The overcoming of a large Peierls-Nabarro stress is the most probable rate-controlling mechanism. Rhombohedral twinning, a significant deformation mode in creep, depends on surface damage for nucleation. The activation energy for rhombohedral twin growth, a function of the applied stress, is substantially lower than that for basal slip. When basal slip and rhombohedral twinning occur concurrently, creep by basal slip results, but the presence of twins can substantially reduce the creep rate.     

Analysis of a Kink Pair Model Applied to a Peierls Mechanism in Basal and Prism Plane Slips in Sapphire (α-Al2O3) Deformed Between 200° and 1800°C

A model based on dislocation glide controlled by the nucleation and propagation of kink pairs in a high Peierls stress crystal is revisited and modified to account for changes in dislocation densities and segment lengths with temperature and stress. It is applied to the critical-resolved shear stress (CRSS) for basal and prism plane slip in sapphire (α-Al₂O₃). According to agreed-upon knowledge on dislocations in sapphire, basal slip and prism plane slip are modeled with undissociated and dissociated dislocations, respectively. In the latter case, partial dislocations move independently. Among a number of sets of fitting parameters, good fits between experimental and modeled CRSS's are obtained in the long segment limit over the whole range of temperatures by making use of physically sound parameters, including a stress dependence of the dislocation density.     

Dislocation Structures in Single-Crystal Al2O3

Chemical polishing and etching techniques were used to reveal the dislocation structures of sapphire and ruby crystals grown by the flame-fusion and flux techniques. The average density of edge dislocations lying in prism planes was 3.0 × 10⁵ per cm², which could be changed only slightly by chromium additions and annealing at 2000°C. An average basal dislocation density of 2 × 10⁵ per cm² decreased 35 to 80% on annealing. Crystal orientation (i.e., angle between the c axis and the growth axis) showed no effect on dislocation density but a pronounced effect on subboundary arrangement and density. The substructure of 0° crystals was more complex than that of 90° crystals; 60° crystals possessed a structure intermediate between 0° and 90°. Principal observations included (1) prismatic and basal slip on all as-grown crystals; (2) profuse basal slip, readily polygonized on annealing; (3) dislocation densities of flux crystals lower than those of Verneuil crystals; and (4) a rare form of basal twinning, composition plane , on all flux crystals.     

Deformation of Hyperstoichiometric UO2 Single Crystals

Hyperstoichiometric UO₂ single crystals having O/M ratios from 2.06 to 2.10 were deformed in compression. The active slip plane for deformation, as evaluated from slip traces, has an orientation between (112) and (111). The critical resolved shear stresses for hyperstoichiometric specimens are approximately the same as those for stoichiometric specimens; the dislocation structures, as revealed by transmission electron microscopy, however, are very different and suggest more rapid motion and/or climb of dislocations in the hyperstoichiometric samples. The response to strain rate changes during deformation also reflects the difference in deformation behavior of hyperstoichiometric and stoichiometric crystals.     

Plastic Deformation of Fine-Grained Alumina (Al2O3): II, Basal Slip and Nonaccommodated Grain-Boundary Sliding

Plastic deformation was studied in fine-grained alumina polycrystals (grain sizes 1 to 5 μm); several deformation mechanisms occur simultaneously. This paper is concerned with basal slip and unaccommodated grain-boundary sliding (GBS). The basal slip can give rise to a deformation texture. Cavitation occurs due to the occurrence of both unaccommodated GBS and basal slip, because of the marked plastic anisotropy of alumina.     

Dislocations and Stacking Faults in Ti3SiC2

The ternary carbide Ti₃SIC₂ fabricated by a reactive hot-press route is investigated by transmission electron microscopy. The material consists mainly of large elongated grains with planar boundaries, and is characterized by a low defect density. Dislocations are observed in the grains and at grain boundaries. Perfect dislocations with b = 1/3<1120> lying in (0001) basal planes are present. These basal plane dislocations are mobile and multiply as a result of room-temperature deformation. All of the stacking faults observed lie in the basal planes.     

In Situ Martensitic Transformation in a Ternary MgO-Y2O3-ZrO2 Alloy: I, Transformation in Tetragonal ZrO2 Grains

The martensitic transformation in tetragonal ZrO₂ grains in a ternary MgO-Y₂O₃-ZrO₂ alloy has been studied using in situ observations in the transmission electron microscope. Transformation occurred by the nucleation and growth of monoclinic laths; thermoelastic equilibrium can be maintained at different extents of transformation by continuously varying the applied stress. The product phase was always twinned, but two twinning mechanisms were found-sequential formation of twin-related variants and posttransformation deformation twinning. In one example, a (401)/(410) pair of martensite habit planes led to a (100) conjunction twinning plane.     

Mechanical Behavior of Samhire

The present state of the knowledge of the mechanical behavior of sapphire is reviewed. Sapphire deforms plastically at temperatures above 900°C, the most common mode of deformation being slip on the basal plane in the 〈11     0〉 direction. Under certain conditions, however, slip may occur on prism planes or twinning may occur. A yield point is often observed, which appears to be related to the multiplication of dislocations by a mechanism controlled by the motion of dislocations through the lattice, rather than by the tearing of dislocations from an impurity (or defect) atmosphere. The dynamics of yielding and flow is similar and can be expressed by either of two thermally activated equations. In one, the effect of stress is principally on the pre-exponential factor; in the other, its effect is principally on the activation energy. There are insufficient data to permit a positive decision between the two, or to positively identify the rate-controlling dislocation mechanism. For 60°-oriented crystals fracture generally occurs on a plane approximately normal to the tensile stress and the fracture surface is conchoidal. In the range 1100° to 1500°C, the tensile fracture stress decreases with increase in plastic strain, independent of temperature and strain rate. The mechanism of failure in this case seems to be the interaction of edge dislocations with pre-existing cracks.     

Slip Systems in Al2O3

Crystallographic notation for Al₂O₃ is reviewed, with particular reference to the correct basis to be used in describing slip systems. A Groves-and-Kelly calculation showed that the combination of pyramidal slip on {11¯02}<11¯01> and basal slip on (0001){112¯0} will allow homogeneous deformation of Al₂O₃ polycrystals. Furthermore, operation of either the {101¯1}<1¯011> or the {011¯2}<2¯021> slip system will also satisfy the Von Mises criterion, since each system is capable of 5 independent deformation modes. Electron microscopy of an Al₂O₃ polycrystal deformed ≅5% at 1150°C under a hydrostatic confining pressure confirmed that pyramidal slip had occurred.     

High-Temperature Deformation of Alumina Double Bicrystals

Deformation and strength of alumina double bicrystals fabricated from verneuil-grown stock were studied as functions of temperature (1210° T 1820°C) and strain rate (0.0005 ε 0.05 min^-1). The oriented specimens had c axes parallel or perpendicular to the compressive stress axes; + a axes and c axes were matched and/or mismatched across the (1123) interfaces of the double bicrystals. Undoped ("pure") double bicrystals in which the c axes and stress axis were coincident deformed by rhombohedral twinning and, at T 1550°C, by slip. Double bicrystals containing crystal segments having c axes perpendicular to the stress axis deformed in part by basal kinking. Interfacial impurity additions of mullite or spinel thin films promoted grain-boundary fracture and sliding, whereas "pure" double bicrystals, even at stresses comparable to the ultimate strengths of single crystals in similar orientations, did not exhibit macrosliding of the grain boundary.     

Plastic Deformation of ZrB2 Single Crystals

The active slip planes, the Burgers vector, and the critical resolved shear stress to induce macroscopic deformation in ZrB₂ single crystals were determined. Room-temperature microhardness indentation and high-temperature uniaxial compression loadings were used to induce deformation. Slip occurred in a close-packed α direction on prismatic planes at room temperature and on the basal plane at high temperatures. The high-temperature yield stress and yield drop are discussed in terms of a Widmanstaetten-type precipitate observed in the crystals.     

Molecular Dynamics Computer Simulations of the Interface Structure of Calcium–Alumino–Silicate Intergranular Films between Combined Basal and Prism Planes of α-Al2O3

The interface structures of calcium–alumino–silicate (CAS) glassy intergranular films (IGFs) formed between the combined basal and prism orientations of α-Al₂O₃ crystals were studied using molecular dynamics simulations. Preferential adsorption of specific ions from the IGFs to the contacting surfaces of the alumina crystals was observed. This segregation of specific ions to the interface enables formation of localized, ordered structures between the IGF and the crystal. However, the segregation behavior of the ions is anisotropic, depending on the orientation of the α-Al₂O₃ crystals. The results show that the enrichment of Ca atoms at the basal interface inhibits growth in the 〈0001〉 direction. However, at the (11 2 0) prism plane, Ca ions have little effect on the epitaxial adsorption of Al and O ions from the IGF onto the (11 2 0) surface. Increasing alumina concentration in the glassy IGF enhances adsorption of Al ions onto the prism surface, with little effect on the basal surface, indicating the tendency of growth in the 〈11 2 0〉 direction on the prism plane, but limited growth on the basal plane. These results are consistent with the experimental data regarding anisotropic grain growth in alumina sintered in the presence of CAS IGFs.     

Kinking and Cracking Caused by Slip in Single Crystals of Silicon Carbide

α-SiC single crystals were compressed parallel to the basal plane, (0001), at temperatures between 900° and 1500°C. Plastic deformation by slip on the basal planes which accompanied kinking occurred above 1000°C. At kink boundaries, two kinds of cracks were observed. One was the cracks elongated parallel to the basal plane. This kind of crack was initiated by the tensile stress produced by piled-up dislocations on the basal planes against a kink boundary. The other was on a kink boundary, and was induced by the stress of dislocations, heterogeneously distributed on the kink boundary. The initiation of cracks produced by dislocations was considered to be a possible cause of fracture in polycrystalline SiC at high temperatures.     

Surface Structure in Corundum: I, Etching of Dislocations

Triangular etch pits, corresponding to the intersection of individual edge dislocations with the surface, have been observed in corundum single crystals after about 5 minutes of immersion in boiling phosphoric acid. Dislocations of both the (0001), (1120) and (1210), (1010) slip systems (where reference is made to the slip plane and slip direction, respectively) have been detected by this method. Edge dislocations of the (0001), (1120) system etched on surfaces close to and including the (1011) and {2021} planes. Dislocations of the {1210}, (1010) systems etched on the basal (0001) plane. The orientation dependence and technique of etching is described. The agreement with the Nye formula and with some of the expected properties of dislocations is cited as evidence that individual edge dislocations are actually detected. Typical photomicrographs of the etched surface in as-received, deformed, flame-polished, and polygonized crystals are shown. The dislocation structure produced in basally deformed crystals was found to depend critically on the constancy of the temperature during deformation. Crystals held at 2000°C. during bending exhibited dislocations arrayed in rows in the slip planes in good agreement with the Nye formula. Crystals bent while cooling (quench-bent) had about twice as many dislocations as predicted by the Nye formula and these were distributed randomly. The possibility of vacancy condensation as a method for dislocation generation in quench-bent crystals is discussed.     

Decoration of Dislocations by the Precipitation of Alumina in MgO · 2.9Al2O3 Spinel

A thermal etching technique is developed to reveal dislocations in MgO · nAl₂O₃ (n=2.9) single crystals decorated by Al₂O₃ precipitation. Large plastic deformation leads to a larger density of thermal etch pits. Also, dense arrays of pits, parallel to the traces of slip planes with a surface, are observed around a Vickers identation. The cracks developed by an indentation run selectively along the 〈100〉 directions and accompany dislocations arrayed in the possible slip planes.     

Anisotropic Calcium Segregation to the Surface of Al2O3

The surface enrichment of Ca on various crystalloraphic planes of CaO-doped sapphire has been measured as a function of annealing temperature using Auger electron spectroscopy (AES). Strong Ca enrichment was found on the (10 1 0) prism plane at ≥1300°C, whereas no evidence or Ca segregation could be observed on the (0001) basal plane up to 1500°C. The surface enrichment factor estimated at 1300°C was at least 3 × 10³ for the prism plane, while that for the basal plane was below 50, which corresponds to the detectability limit of AES. The Ca segregation to the prism plane was uniform and limited to the surface monolayer; an apparent heat of segregation determined in the range of 1300° to 1500°C was–169 kJ/mol. Low-energy electron diffraction studies of annealed surfaces revealed that Ca segregation was concurrent with a two-dimensional surface phase transition. The anisotropic segregation behavior of Ca may explain why CaO is not an effective additive for alumina sintering.     

Plastic Deformation of Fine-Grained Alumina (Al2O3): I, Interface-Controlled Diffusional Creep

Plastic deformation in fine-grained alumina polycrystals (grain size 1 to 15 μm) was studied. At least three distinct deformation mechanisms are important: diffusional creep, basal slip, and unaccommodated grain-boundary sliding. The first and most important of these processes is addressed in this paper. Analysis of the deformation dynamics suggests that both lattice and grain-boundary diffusion are important in the diffusional creep. Aluminum, rather than oxygen, lattice and grain-boundary diffusion are rate-controlling because oxygen diffusion is very slow in the lattice but very rapid in grain boundaries. Significantly, the diffusional creep can become interfacecontrolled at low stresses, causing the often-reported non-Newtonian creep behavior of fine-grained alumina.     

Prismatic Slip of A12O3 Single Crystals Below 1000°C in Compression Under Hydrostatic Pressure

Alumina single crystals were compressed perpendicular to the [0001] axis at a constant strain rate between 20° and 950°C. At r>200°C, failure was suppressed by_hydrostatic pressures of 500 to 1500 MPa. Prismatic slip {1120}〈1100〉 was deduced from optical observations of the lateral surfaces and from stress-optical features in thin sections cut from the specimens. The critical resolved shear stress (CRSS) decreased rapidly with increasing temperature, from a maximum of ∼3000 MPa at 200°C (strain rate 2±10-⁻⁵ s⁻¹). A simple linear law can be fitted with the logarithm of the CRSS as a function of temperature, up to 1800°C. The rate-controlling mechanism for dislocation glide is likely to be either the Peierls barrier or barriers due to dissociation out of the glide plane.     

Dislocation-Induced Softening of MgO·2.9Al2O3 Single Crystals

Magnesium aluminate spinel (MgO·2.9Al₂O₃) single crystals were deformed in compression along the [001] direction at temperatures between 1100° and 1500°C. Dislocations introduced by plastic deformation were observed by transmission electron microscopy. These dislocations lead to plasticity at a temperature where undeformed spinel has no ductility. Further, room-temperature Vickers hardness decreases after plastic deformation at 1500°C.     

Plastic Deformation and Solid-Solution Hardening of Y2O3-Stabilized ZrO2

Fully stabilized cubic ZrO₂ single crystals containing various Y₂O₃ concentrations were deformed at 1400°C in air. The orientation chosen favored (001)(110) slip, which was confirmed by slip-trace analysis and transmission electron microscopy; (111)(110) slip could also be activated. The yield and flow stresses increased with increasing Y₂O₃ concentration, and stress-strain curves were dominated by a region of zero work hardening from very small strains for all compositions.