High-angle grain boundaries are generally deemed necessary for superplasticity in metals. In polycrystalline materials the grain boundary character must be described in terms of a probability distribution rather than by a single parameter, and little has been reported on the relationship between this distribution and fine-grain superplasticity. For aluminum alloys that exhibit continuous recrystallization the results of computer-aided electron backscatter diffraction analysis have shown that bimodal grain boundary disorientation distributions are present in as-processed material and persist during subsequent annealing. Such distributions may be simulated by computer methods based on a model of the microstructure which assumes that deformation banding occurs during deformation processing. High-angle boundaries (≥30°) develop in association with deformation banding while boundaries of lower disorientation (<30°) develop by dislocation reaction within the bands. Improved understanding of the grain boundary types associated with various microstructural transformation mechanisms will aid the design of processes to produce superplastic microstructures.

Microstructures of a binary Nb-15.8at%Al alloy ingot were controlled by isothermal forging and heat treatment to produce equiaxed, fine grains of Nb3Al and Nb solid solution (Nb33). Nb3Al/Nb33 two phase alloy (in-situ composite) is found to exhibit superplasticity especially when one of the constituent phases, Nb33, is supersaturated. During superplastic deformation Nb33 transforms to Nb3Al, and Al content in Nb33 decreases. After superplastic deformation the microstructure consisting of equiaxed grains is left unchanged, although a slight grain growth is observed. It is suggested that stress induced by grain boundary sliding is effectively accommodated through dislocation glide and climb in the soft Nb33

An Al-4Mg-0.3Sc alloy, aged at 280°C for 8 hours and cold rolled to a 70% reduction, exhibited dynamic recrystallization during superplastic forming at 460°C and at a strain rate of 10−3sec−1. To understand the progression of recrystallization during forming, specimens were deformed under these same conditions to 0.1, 0.2, 0.4 and 0.8 true strain and studied postmortem using optical microscopy, transmission electron microscopy and orientation imaging microscopy. The microstructural evolution that occurred between each strain state was directly observed during deformation experiments at a nominal temperature of 460°C in the transmission electron microscope. These in-situ experiments showed the migration, coalescence, disintegration and annihilation of subboundaries. This combination of post-mortem analysis of specimens strained in bulk with real time observations made during these in-situ experiments allows the mechanisms operating during dynamic continuous recrystallization to be ascertained.

Identical Al-Mg-Mn-Sc alloys without and with 0.034-wt% Sn additions were fabricated, heat-treated, and tensile tested in a fine-grain (d < 6 pm) condition at four strain rates from 10−2 to 10−4 s−1 and at temperatures from 723K to 823K. Alloys with Sn additions exhibited reduced failure strains at 723K but higher failure strains at 823K for the slowest strain rates. The effect of Sn on flow stress, activation energy for flow stress, and strain rate exponent was explored and was found to be small. The main effect of Sn was suggested to be in reducing cavitation by allowing a redistribution of stress at critical hetero-junctions in the alloys.

The superplastic deformation behavior of a quasi-single phase Zn-0.3 wt.% Al and a microduplex Zn-22 wt.% Al eutectoid alloy has been investigated in this study within the framework of the internal variable theory of structural superplasticity (SSP). Load relaxation and tensile tests were conducted at room temperature for quasi-single phase alloy and at 200°C for eutectoid alloy. The flow curves obtained from load relaxation tests on superplastic Zn-Al alloys were shown to consist of the contributions from interface sliding (IS) and the accommodating plastic deformation due to dislocation activities. The IS behavior could be described as a viscous flow characterized by the power index value of Mg = 0.5. In the case of quasi-single phase Zn-0.3 wt.% Al alloy with the average grain size of 1 µm, a large elongation of about 1400 % was obtained at room temperature. In a relatively large-grained (10 µm) single-phase alloy, however, grain boundary sliding (GBS) was not expected from the analysis based on the internal variable theory of SSP.

This paper will describe the generation of micro- and sub-microcrystalline structures in two Ni-based alloys that are typically strengthened by phases, such as γ′ and γ″+δ. The relationship between the superplastic behavior and microstructure will be discussed. High strain deformation processing in the temperature range of 0.9 Tm to 0. 6Tm results in reduction of the initial coarse-grained structure (>100 µm) to a range of structures including microcrystalline (MC) (grain size <10 µm) and sub-microcrystalline (SMC) (grain size <1 µm) with increasing deformation. The influence of alloy chemistry and constituent phases on dynamic and static recrystallization is considered, and their effect on grain refinement is described. Low-temperature and high strain rate superplasticity can be observed in dispersionstrengthened alloys with SMC structures. It was established that in dispersion-hardened Ni alloys with SMC structures, superplasticity can be observed at temperatures 200-250°C lower than in alloys with MC structure.

During thermal cycling through the α/β phase transformation under the action of a small external biasing stress, Ti alloys exhibit an average deformation stress exponent of unity and achieve superplastic strains. We report tensile experiments on Ti-6Al-4V with an applied stress of 4.5 MPa, aimed at understanding the failure processes during transformation superplasticity. The development of cavities is assessed as a function of superplastic elongation, and macroscopic neck formation is quantified at several levels of elongation by digital imaging techniques. The effects of thermal inhomogeneity on neck initiation and propagation are also elucidated experimentally.

Cavitation caused by superplastic straining of a fine-grained Al-Mg-Mn-Cu alloy under uniaxial tension has been systematically evaluated. Tensile tests were conducted in the strain-rate range of 10−4s−1 to 10−2s−1 and in the temperature range of 450°C to 550°C. Measurements of the number and size of cavities were made by image analysis through optical microscopy on tested specimens. With increasing imposed strain, the cavity population density increases. Cavity growth has been found to be primarily due to the plastic deformation of the matrix. These results are characterized by the total volume fraction of cavities which is found to increase exponentially with strain. However, the dependencies of cavity volume fraction on strain-rate and temperature are not straightforward and the notion of just a few large cavities controlling the total cavity volume is not always true. Attempts to explain these complex dependencies have been carried out based on the concepts of debonding between the matrix and non-deformable particles, the continuous nucleation of new cavities, and plasticity-based cavity growth for large cavities.

Cavitation behaviors related to ferrous primary crystals have been investigated at a temperature of 653 K and a strain rate of 10−3/s for Al-4.5%Mg-0.05%Fe and Al-4.5%Mg-0.2%Fe alloys which have a grain size of 50;Lm. The alloys constantly exhibited a large elongation-to-failure above 300% at the temperature of 653 K and strain rate of 10−3/s. Cavitation was increased by increasing the iron content. Most cavities were nucleated at the interface between the ferrous primary crystal and matrix and elongated parallel to the tensile direction. The experimental critical diameter of the primary crystal, above which cavity is nucleated, was 1.5 µm at the grain boundary and 0.5µm at grain interior, which were very close to double the critical diffusion length.

The superplastic flow behavior of a near-γ titanium aluminide (Ti-45.5Al-2Cr-2Nb) is determined under uniaxial tension in as-rolled or rolled-and-heat treated conditions (1177°C/4 hr or 1238°C/2 hr). Cavitation characteristics, including cavity growth rates, are established via isothermal, constant strain rate tests conducted at 10−4 to 10−2 s−1 and temperatures between 900°C and 1200°C. Differences in cavitation as a function of initial structure, strain, strain rate and temperature are noted. Cavity growth is found to be largely plasticity controlled. Experimental growth rates are compared with equations that predict rates as a function of strain rate sensitivity. Although the equations assume no coalescence and no nucleation of new cavities, which are experimentally observed, they are useful in predicting actual growth rates.

Highly deformable ceramics can be created with the addition of intergranular silicate phases. These amorphous intergranular phases can assist in superplastic deformation by relieving stress concentrations and minimizing grain growth if the appropriate intergranular compositions are selected. Examples from 3Y-TZP and 8Y-CSZ ceramics are discussed. The grain boundary chemistry is analyzed by high resolution analytical TEM is found to have a strong influence on the cohesion of the grains both at high temperature and at room temperature. Intergranular phases with a high ionic character and containing large ions with a relatively weak bond strength appear to cause premature failure. In contrast, intergranular phases with a high degree of covalent character and similar or smaller ions than the ceramic and a high ionic bond strength are the best for grain boundary adhesion and prevention of both cavitation at high temperatures and intergranular fracture at room temperature.

The high temperature deformation behavior of a 3mol% yttria-stabilized tetragonal zirconia (3Y-TZP) is examined. The analysis of creep strain rate, which was monitored directly with an optical extensometer and corrected for the current grain size, reveals a sigmoidal feature in the true stress-creep rate relationship. At lower stresses, a stress exponent n of ∼1.6 incorporated with a grain size exponent of 2.0 suggests the intervention of a lattice diffusion creep mechanism. For higher stresses where n ∼2.7, evidence of intragranular dislocation activities suggests that dislocations may play an important role in the accommodation process for grain boundary sliding in 3Y-TZP.

Steady-state creep and joining of alumina/zirconia composites containing alumina volume fractions of 20, 60, and 85% have been investigated between 1250 and 1350°C. Superplasticity of these compounds is controlled by grain-boundary sliding and the creep rate is a function of alumina volume fraction, not grain size. Using the principles of superplasticity, pieces of the composite have been joined by applying the stress required to achieve 5 to 10% strain to form a strong interface at temperatures as low as 1200°C

Flow data are reported for a superplastic yttria-stabilized tetragonal zirconia containing 3 mol % of Y2O3 (termed 3Y-TZP). The data are analyzed using a model for interface-controlled diffusion creep and the results are compared with published data for other samples of 3Y-TZP.

The creep characteristics of a high purity superplastic Y-TZP/Al2O3 composite were studied. The test samples had a uniform initial grain size of essentially equiaxed grains and the phase distribution was also uniform. Creep tests were conducted at elevated temperatures in tension and measurements were taken after testing to determine the average size and shape of the grains. The creep curves showed the existence of a primary stage of creep and then a transition into a steady-state region where the strain rate remained reasonably constant. Observations by scanning electron microscopy revealed an elongation of the alumina grains with the grain strain essentially matching the overall strain within the sample. There was some grain growth after testing at the lower stresses. Preliminary observations using an atomic force microscope revealed direct evidence for the occurrence of some grain boundary sliding within the samples. The results are compared with earlier data reported for Y-TZP/Al2O3 composites and they are analyzed using the interface reaction-controlled diffusion creep model.

The different scales of plastic flow in silicon nitride were investigated either by indentation experiments and compression under hydrostatic pressure in the 20-850°C temperature range, and by stress relaxation and creep above 1350°C. [0001], 1/3<11-20> and 1/3<11-23> dislocations were evidenced by Transmission Electron Microscopy (TEM) in the low temperature range. Cross-slip events in {10-10} prismatic planes were observed at temperature as low as 20°C by Atomic Force Microscopy (AFM) on micro-hardness indents. By increasing the temperature, the deviation plane becomes {11-20} prismatic planes. The easiest slip system is by far the [0001]{10-10} system. Above 1350°C, the creep strain could be fitted by the sum of a transient component, εt=ε∞[1-exp-(t/τc)bc], where τc reflects the duration of the transient creep stage, and bc is between 0 and 1, and a stationary component, εs=εst =Aσnt, where σ is the stress and n is the stress exponent. The increase of ε∞ with temperature is interpreted on the basis of the formation of liquid intergranulary phases above 1400°C by progressive melting of some of the grains. A creep exponent of 1.8 was determined. A single value could hardly be given to the activation energy since an S-shape curve was observed in the In εs versus l/T plot, as for most glasses over large temperature ranges. The stress relaxation kinetics was found to follow the Kohlrausch-Williams-Watt expression: σ/σo=exp [-(t/τr)br], where br ranges between 0 (solid state) and I (liquid state) and τr is a characteristic relaxation time constant. As in the case of glasses, τr decreases rapidly whereas br increases from about 0.2 to 0.7 as the temperature increases from 1400 to 1650°C. But again, it is very difficult to get a single value for the activation energy from the In τr versus 1/T plot.

Alumina bicrystals were fabricated by a hot joining technique at 1500°C in air to obtain ten kinds of [0001] symmetric tilt grain boundaries which included small angle, CSL and high angle grain boundaries. Their grain boundary structures were investigated by high-resolution electron microscopy (HREM), and the respective grain boundary energies were systematically measured by a thermal grooving technique. It was found that grain boundary energy strongly depended on the grain boundary characters, e.g., there were large energy cusps at low Σ CSL grain boundaries. But, main part of grain boundary energy is likely to be due to the strain energy around the grain boundary, and the contribution of atomic configuration is not so large. Small angle grain boundaries were consisted of an array of partial dislocation with Burgers vector of 1/3[1100] to form the stacking faults between the dislocations. The behavior of grain boundary sliding was also investigated for typical grain boundaries by high-temperature creep test at 1400°C. As the result, the occurrence of grain boundary sliding was found to depend on the grain boundary atomic structure.

The compression and the tension tests of liquid-phase sintered β-SiC fabricated by hot-pressing using ultra fine powders were performed at 1973 K ∼ 2048 K in N2 atmosphere. Amorphous phases were observed at the grain boundaries and at multi-grain junctions in the assintered material. Strain hardening was observed under all experimental conditions. Stress exponents in the compression test were from 1.7 to 2.1 in the temperature ranging from 1973 K to 2023 K. A maximum tensile elongation of 170 % was achieved at the initial strain rate of 2 Χ 10−5 s−1 at 2048 K.

Bulk amorphous alloys have many unique properties, e.g., superior strength and hardness, excellent corrosion resistance, reduced sliding friction and improved wear resistance, and easy formability in a viscous state. These properties, and particularly easy formability, are expected to lead to applications in the fields of near-net-shape fabrication of structural components. Whereas large tensile ductility has generally been observed in the supercooled liquid region in metallic glasses, the exact deformation mechanism, and in particular whether such alloys deform by Newtonian viscous flow, remains a controversial issue. In this paper, existing data are analyzed and an interpretation for the apparent controversy is offered. In addition, new results obtained from an amorphous alloy (composition: Zr–10Al–5Ti–17.9Cu–14.6Ni, in at. %) are presented. Structural evolution during plastic deformation is particularly characterized. It is suggested that the appearance of non-Newtonian behavior is a result of the concurrent crystallization of the amorphous structure during deformation.