Microstructural influences on superplasticity in Ti-6AI-4V

The strong dependence of the superplastic behavior of metals and alloys on grain size has been demonstrated, and it is now well known that a fine grain size is normally a requirement for superplasticity. However, the microstructure of certain alloy systems such as Ti-6A1-4V cannot always be adequately characterized by a single parameter such as grain size. In two-phase α β alloys such as Ti-6A1-4V, other microstructural parameters such as volume fractions of the two phases, grain aspect ratio, grain size distribution and crystallographic texture may also influence superplasticity. For example, if “grain switching” is an important deformation mechanism in superplastic flow as suggested by Ashby and Verall, then factors such as grain aspect ratio and range of grain sizes would be expected to have an effect on superplastic behavior. In this study, these microstructural features were determined for several different heats of Ti-6Al-4V, and the corresponding superplastic properties were evaluated in terms of their fully characterized microstructure. The flow stress as a function of strain rate, strain rate sensitivity exponent (m) as a function of strain rate and total elongation on properties were found to be strongly influenced by microstructural parameters such as grain aspect ratios, grain size and grain size distribution.     

Superplasticity of an aluminum-lithium 1420 alloy in various structural states

The superplasticity of Al-Li-Mg alloy 1420 with a grain size of 0.3–20 μm has been studied in various structural states. A nonlinear dependence of the superplastic elongation on the grain size is revealed. The optimum temperatures and strain rates are determined for nanocrystalline and submicrocrystalline alloys: they have large elongations (1200–1500%), high strain-rate sensitivity coefficients (higher than 0.45), and low activation energies (60–70 kJ/mol). The existence of an optimal grain size for reaching the maximum strain under structural superplasticity conditions is explained using a theoretical model proposed in this work.     

New aspects on the superplasticity of fine-grained 7475 aluminum alloys

Thermomechanical processes were developed which give fine grain sizes of 6 and 8 μm in the 7475 Al alloy. Superplastic properties of this material were evaluated in the temperature range of 400 °C to 545 °C over the strain-rate range of 2.8 x 10^-4 to 2.8 X 10^-2 s^-1. The maximum ductility exhibited by the alloy was approximately 2000 pct, and optimum superplasticity was achieved at a strain rate of 2.8 X 10^-3 s^-1 which is higher by an order of magnitude than other 7475 Al alloys. This result is attributed to the presence of fine dispersoids which maintain the fine grain size at high homologous temperatures. The flow stress and strain-rate sensitivity strongly depend on the grain size. The superplastic 7475 Al alloy has strain-rate sensitivities of 0.67 (6 μm) and 0.5 (13 μm) and an activation energy which is similar to the one for grain boundary diffusion of aluminum. Microstructural investigation after superplastic tests revealed zones free of dispersoid particles at grain boundaries primarily normal to the tensile direction. These dispersoidfree zones (DFZs) appear even after 100 pct elongation and are occasionally as large as 5 μm across. This result demonstrates the importance of diffusional flow in superplastic deformation of the fine-grained 7475 Al alloy especially at low elongations.     

An evaluation of the flow behavior during high strain rate superplasticity in an Al-Mg-Sc alloy

An Al-3 pct Mg-0.2 pct Sc alloy was fabricated by casting and subjected to equal-channel angular pressing to reduce the grain size to ∼0.2 μm. Very high tensile elongations were achieved in this alloy at temperatures over the range from 573 to 723 K, with elongations up to >2000 pct at temperatures of 673 and 723 K and strain rates at and above 10⁻² s⁻¹. By contrast, samples of the same alloy subjected to cold rolling (CR) yielded elongations to failure of <400 pct at 673 K. An analysis of the experimental data for the equal-channel angular (ECA)-pressed samples shows consistency with conventional superplasticity including an activation energy for superplastic flow which is within the range anticipated for grain boundary diffusion in pure Al and interdiffusion in Al-Mg solid solution alloys.     

Effects of microstructural evolution on superplastic deformation characteristics of a rapidly solidified Al-Li alloy

This study is concerned with the effects of microstructural modification on superplastic deformation characteristics of a rapidly solidified (RS) Al-3Li-1Cu-0.5Mg-0.5Zr (wt pct) alloy. This Al-Li alloy has a very fine grain structure desirable for improved superplasticity. The results of superplastic deformation indicated that the alloy exhibited a high superplastic ductility, e.g., elongation of approximately 800 pct, when deformed at temperatures above 500 °C and at the strain rates of 10⁻²/s to 10⁻¹/s. Such a high strain rate is quite advantageous for the practical superplastic forming application of the alloy. Stress-strain rate curves were obtained by performing a series of load relaxation tests in the temperature range from 460 °C to 520 °C in order to examine the superplastic deformation behavior and to establish its mechanisms. The stress-strain rate curves could be separated into two parts according to their respective physical mechanisms, i.e., grain matrix deformation and grain boundary sliding, as was proposed in a new superplasticity theory based on internal deformation variables. The microstructural evolution during superplastic deformation was also analyzed by using transmission electron microscopy. During superplastic deformation, grains were kept fine and changed into equiaxed ones due to the presence of fine secondary phase particles and the continuous recrystallization due to the development of subgrains. Consequently, the rapidly solidified (RS) alloy showed much improved superplasticity compared to the conventional ingot cast 8090 alloy.     

An evaluation of the flow behavior during high strain rate superplasticity in an Al−Mg−Sc alloy

An Al-3 pct Mg-0.2 pct Sc alloy was fabricated by casting and subjected to equal-channel angular pressing to reduce the grain size to ∼0.2 μm. Very high tensile elongations were achieved in this alloy at temperatures over the range from 573 to 723 K, with elongations up to >2000 pct at temperatures of 673 and 723 K and strain rates at and above 10⁻² s⁻¹. By contrast, samples of the same alloy subjected to cold rolling (CR) yielded elongations to failure of <400 pct at 673 K. An analysis of the experimental data for the equal-channel angular (ECA)—pressed samples shows consistency with conventional superplasticity including an activation energy for superplastic flow which is within the range anticipated for grain boundary diffusion in pure Al and interdiffusion in Al−Mg solid solution alloys. MINORU NEMOTO, formerly Professor, Department of Materials Science and Engineering, Faculty of Engineering, Kyushu University.     

Characterization and analysis of low-temperature superplasticity in 8090 Al-Li alloys

The 8090 Al-Li alloys, after a special thermomechanical process (TMP), exhibited low-temperature superplasticity (LTSP) from 350 °C to 450 °C and behaved differently from the conventional high-temperature superplasticity (HTSP). The LTSP sheets after ~700 pct elongation at 350 °C and 8 × 10⁻⁴ s⁻¹ still possessed fine “(sub)grains” 3.7 μm in size and narrow surface Li-depletion zones 11 μm in width, resulting in a post-SP T6 strength of ~500 MPa, significantly higher than that of the 8090 alloys tested at normal superplastic temperature of 525 °C or above. Examination from the movement of surface marker lines in LTSP samples confirmed the role of grain boundary sliding (GBS), coupled with grain rotation and migration. During the initial stage (<150 pct), GBS along certain higher-angled boundaries was proceeded along a plane ±45 deg with respect to the sample surface. With increasing straining, sliding between individual grains or grain groups was observed on other planes, forming a zigzag morphology. Transmission electron microscopy (TEM) observations revealed appreciable dislocation activities, suggesting the involvement of dislocation creep. The tensile behavior and deformation mechanisms of the HTSP and LTSP sheets were investigated and analyzed over the strain rates range 10⁻⁵ to 10⁻² s⁻¹. The strain-rate sensitivity(m value) for the LTSP and HTSP materials was found to be ~0.33 and 0.50, respectively. The activation energy was extracted to be 92 kJ/mole for the LTSP sheets and to be 141 kJ/mole for the HTSP sheets. Based upon these results, the primary deformation and accommodation mechanisms for the HTSP and LTSP sheets are GBS and dislocation creep, respectively.     

Effect of friction stir processing on the kinetics of superplastic deformation in an Al-Mg-Zr alloy

The effect of friction stir processing on the superplastic behavior of extruded Al-4Mg-1Zr was examined at 350 °C to 600 °C and at initial strain rates of 1×10⁻³ to 1 s⁻¹. A combination of a fine grain size of 1.5 μm and high-angle grain boundaries in the friction stir-processed (FSP) alloy led to considerably enhanced superplastic ductility, much-reduced flow stress, and a shift to a higher optimum strain rate and lower optimum temperature. The as-extruded alloy exhibited the highest superplastic ductility of 1015 pct at 580 °C and an initial strain rate of 1×10⁻²s⁻¹, whereas a maximum elongation of 1280 pct was obtained at 525 °C and an initial strain rate of 1×10⁻¹s⁻¹ for the FSP alloy. The FSP alloy exhibited enhanced superplastic deformation kinetics compared to that predicted by the constitutive relationship for superplasticity in fine-grained aluminum alloys. A possible origin for enhanced superplastic deformation kinetics in the FSP condition is proposed.     

Superplasticity and residual tensile properties of a microduplex copper-nickel-zinc alloy

Structural superplasticity in two phase alloys of the copper-nickel-zinc system (nominal composition in wt. pct Cu-15Ni-38 Zn-0.2 Mn) occurs over a wide range of strain rates in the temperature range 850 to 1050∮F (454 to 565°). The upper temperature limit for super-plastic behavior in this system is determined by the reversion of the fine-grained two-phase structure to a single phase structure in which extensive grain growth is possible. Residual room temperature tensile properties and microstructure of the microduplex alloy after superplastic straining have been studied as a function of test temperature and total super-plastic strain. At test temperatures sufficiently removed from the phase transformation temperature, the high tensile properties and fine microstructure of the starting material are essentially retained after superplastic strains approaching 200 pct. In the immediate vicinity of the phase transformation temperature, rapid degradation of the microduplex structure occurs during superplastic deformation with a consequent severe degradation of the residual room temperature tensile properties. Formerly with The International Nickel Company, is now with Gulf Energy and Environmental Systems, Materials Science Department, P. O. Box 608, San Diego, Calif. 92112.     

An investigation of superplasticity in a thermomechanically processed U-6nb (α + γ2) alloy

A uranium-6 niobium alloy was shown to exhibit superplasticity. A thermomechanical processing (TMP) sequence was used to develop the ultrafine grain size essential for superplastic behavior. Strain-rate sensitivity, maximum elongation, and flow curve data indicated that this alloy is superplastic above the monotectoid temperature (647 °C) in the equilibrium γ₁, single-phase, temperature regime. The existence of superplasticity in the single-phase temperature regime was explained by the presence of metastable γ₂ at these higher temperatures. Sluggish niobium diffusion and the resultant slow dissolution kinetics were shown to be responsible for this anomalous “single-phase” superplastic behavior. An engineering elongation of 658 pct was obtained at 685 °C for a constant true strain rate of 2.5 × 10^-4 s^-1 which required an initial flow stress of only 2.8 MPa. A grain growth kinetic study, along with flow curve information, has also shown that superplastic forming (SPF) must be completed within 2 hours at 670 °C to obtain maximum ductility with the lowest forming pressure.     

Microstructural aspects of superplasticity

This short review summarizes the contribution of microstructural studies to the present understanding of the deformation mechanisms operating during superplastic deformation. A background summary is included that describes the major features of superplasticity, the relevant deformation theories, and the requirements for successful microstructural studies. However, most of the paper is concentrated on a discussion of the microstructural evidence in the literature on two types of material. The first is a representative group of modern commercial nickel, aluminum, and magnesium alloys. The second is the Zn-Al eutectoid, a member of the well characterized “classical” group of superplastic materials based upon eutectic or eutectoid compositions. The importance of dislocation motion at maximumm is emphasized, both as an accommodation mechanism for grain boundary sliding and directly in response to the applied stress. However, it is shown that, in IN100 and Supral 150, other processes occur simultaneously, including recrystallization and diffusion. This paper is based on a presentation made at the symposium “On the Mechanical, Microstructural and Fracture Processes in Superplasticity” held at the annual meeting of the AIME in Pittsburgh, PA on October 7, 1980 under the sponsorship of the Flow and Fracture Activity of the Materials Science Division of ASM.     

A model for subgrain superplastic flow in aluminum alloys

Aluminum alloys that contain low angle boundaries exhibit different superplastic behavior than alloys consisting of high angle boundaries. On a relative basis, the low angle boundaries increase the flow stress, but impart a greater resistance to cavitation; the strain-rate sensitivity of this material is generally smaller and the change in the strain-rate sensitivity with strain rate shows a minimum instead of a maximum as observed in the large angle boundary materials. As a result, the subgrain material can be deformed to large tensile strains at fast strain rates. A kinetic model for subgrain superplasticity that invokes a balance between the arrival and emission rates of dislocations at low angle boundaries is presented. It explains several features of subgrain superplasticity. It also explains why ultrafine dispersoids of intermetallics appear to stabilize the subgrain structure in aluminum. Early work on the correlation between flow stress and the subgrain size in dynamic recrystallization of metals may also be consistent with the model.     

单相组织金属间化合物的超塑性行为

在一定条件下具有单相微观组织的L12型[Ni3Al,Ni3(Si,Ti),Co3Ti],L10型（TiAl)和B2型（FeAl,Fe3Al,NiAl)金属间化合物均表现出超塑性行为。其中,L12型和L10型金属间化合物的超塑性变形机制为晶界的滑移,而B2型金属间化合物的超塑性变形则来自于变形过程中发生的动态回复及再结晶,超塑性变形机制的多样性是由于金属间化合物在微观组织及位错结构上（如反向畴界能,层错能和化学成分差异,超位错及界面位错等）比普通金属合金要复杂得多。     

High strain rate superplasticity of a 25 Wt Pct Cr-7 Wt Pct Ni-3 Wt Pct Mo-0.14 Wt Pct N duplex stainless steel

Effects of prior thermomechanical treatments on the superplasticity of a 25 wt pct Cr-7 wt pct Ni-3 wt pct Mo-0.14 wt pct N δ/γ duplex stainless steel have been studied by means of hot tensile testing with constant crosshead speeds. The objective is to increase the strain rate suitable for superplasticity. The strain rate is found to be markedly increased by a special prior treatment,i.e., solution treatment at temperatures in the δ single-phase region with subsequent heavy cold-rolling. In hot tensile tests at 1273 K, elongations greater than 1000 and 300 pct were observed at initial strain rates (έ) of 10⁻³ to 10⁻¹ s⁻¹ and 1 x 10⁰ s⁻¹, respectively. The results for strain rates 〈10⁻¹ s⁻¹ can be explained in terms of a structural superplastic effect due to grain refinement. In the case of έ 〉 10⁻¹ s⁻¹, transformation superplastic effects due to γ-phase precipitation from the σ-ferrite matrix are also important, especially in the early stages of deformation. In the equiaxedδ/γ microduplex structures during stable superplastic deformation, there exists a mixture of two different structures,i.e., dislocated and recovered/ recrystallized δ grains with a homogeneous dispersion of dislocation-free γ particles. This result shows that dynamic recrystallization ofδ grains occurs locally and intermittently due to the dispersion of relatively hardγ particles. The apparent average grain growth rate during deformation is small compared to static grain growth, because grain refinement due to dynamic recrystallization reduces the superplasticity-enhanced grain growth.     

High-strain-rate superplasticity in bulk cryomilled ultra-fine-grained 5083 Al

The ductility and creep of bulk ultra-fine-grained (UFG) 5083 Al (grain size ∼440 nm) processed by gas atomization, cryomilling, and consolidation were studied in the temperature range 523 to 648 K. Also, the creep microstructure developed in the alloy was examined by means of transmission electron microscopy (TEM). The ductility as a function of strain rate exhibits a maximum that shifts to higher strain rates with increasing temperature. An analysis of the experimental data indicates that the true stress exponent is about 2, and the true activation energy is close to that anticipated for boundary diffusion in 5083 Al. These creep characteristics along with the ductility behavior of 5083 Al are a reflection of its creep behavior as a superplastic alloy and not as a solid-solution alloy. In addition, the observation of elongations of more than 300 pct at strain rates higher than 0.1 s⁻¹ is indicative of the occurrence of high-strain-rate (HSR) superplasticity. Microstructural evidence for the occurrence of HSR superplasticity includes the retention of equiaxed grains after deformation, the observation of features associated with the occurrence of grain boundary sliding, and the formation of cavity stringers. Grain size stability during the superplastic deformation of the alloy is attributed to the presence of dispersion particles that are introduced during gas spraying and cryomilling. These particles also serve as obstacles for dislocation motion, which may account for the threshold stress estimated from the creep data of the alloy.     

Fabrication of bulk ultrafine-grained materials through intense plastic straining

Ultrafine grain sizes were introduced into samples of an Al-3 pct Mg solid solution alloy and a cast Al-Mg-Li-Zr alloy using the process of equal-channel angular (ECA) pressing. The Al-3 pct Mg alloy exhibited a grain size of ∼0.23 μm after pressing at room temperature to a strain of ∼4, but there was significant grain growth when the pressed material was heated to temperatures above ∼450 K. The Al-Mg-Li-Zr alloy exhibited a grain size of ∼1.2 μm, and the microstructure was heterogeneous after pressing to a strain of ∼4 at 673 K and homogeneous after pressing to a strain of ∼8 at 673 K with an additional strain of ∼4 at 473 K. The heterogeneous material exhibited superplastic-like flow, but the homogeneous material exhibited high-strain-rate superplasticity with an elongation of >1000 pct at 623 K at a strain rate of 10⁻² s⁻¹. It is concluded that a homogeneous microstructure is required, and therefore a high pressing strain, in order to attain high-strain-rate superplasticity (HSR SP) in ultrafine-grained materials. This article is based on a presentation made in the symposium “Mechanical Behavior of Bulk Nanocrystalline Solids,” presented at the 1997 Fall TMS Meeting and Materials Week, September 14–18, 1997, in Indianapolis, Indiana, under the auspices of the Mechanical Metallurgy (SMD), Powder Materials (MDMD), and Chemistry and Physics of Materials (EMPMD/SMD) Committees.     

Structural superplasticity in a fine-grained eutectic intermetallic NiAl−Cr alloy

A rapidly solidified and thermomechanically processed fine-grained eutectic NiAl−Cr alloy of the composition Ni₃₃Al₃₃Cr₃₄ (at, pct) exhibits structural superplasticity in the temperature regime from 900°C to 1000°C at strain rates ranging from 10⁻⁵ to 10⁻³ s⁻¹. The material consists of a B2-ordered intermetallic NiAl(Cr) solid solution matrix containing a fine dispersion of bcc chromium. A high strain-rate-sensitivity exponent of m=0.55 was achieved in strain-rate-change tests at strain rates of about 10⁻⁴ s⁻¹. Maximum uniform elongations up to 350 pct engineering strain were recorded in superplastic strain to failure tests. Activation energy analysis of superplastic flow was performed in order to establish the diffusion-controlled dislocation accommodation process of grain boundary sliding. An activation energy of Q _c=288±15 kJ/mole was determined. This value is comparable with the activation energy of 290 kJ/mole for lattice diffusion of nickel and for ⁶³Ni tracer selfdiffusion in B2-ordered NiAl. The principal deformation mechanism of superplastic flow in this material is grain-boundary sliding accommodated by dislocation climb controlled by lattice diffusion, which is typical for class II solid-solution alloys. Failure in superplastically strained tensile samples of the fine-grained eutectic alloy occurred by cavitation formations along NiAl‖‖Cr interfaces.     

Enhanced superplasticity and strength in modified Ti-6AI-4V alloys

Although Ti-6A1-4V displays extensive superplasticity at 1200 K, lower superplastic forming temperatures are desirable. A study was conducted with the goal of modifying the composition of the Ti-6A1-4V alloy to lower the optimum superplastic forming temperature. Computer modeling results and previous experimental data suggested that additions to Ti-6A1-4V of beta-stabilizing elements which have high diffusivity in the beta-phase would permit lower superplastic forming temperatures. A series of modified alloys with 2 wt pct additions of Fe, Co, and Ni was prepared for experimental evaluation. The modified alloys achieved desirable microstructures for superplasticity at 1088 K,i.e., the grain size was approximately 5 μm and roughly equal volume fractions of the alpha- and beta-phases were present at the deformation temperature. The superplastic properties of the modified alloys were measured at 1088 K and 1144 K. The modified alloys produced values of flow stress, strain rate sensitivity, and total elongation at 1088 K approaching those of the base Ti-6A1-4V alloy at its standard superplastic forming temperature of 1200 K. In addition to lowering the superplastic forming temperature, the β-stabilizing additions also increased room temperature strength levels above those normally found for Ti-6A1-4V. Based on the room temperature and elevated temperature tensile properties, addition of selected beta-stabilizing elements to Ti-6A1-4V simultaneously raises resistance to deformation at room temperature and lowers resistance to deformation at elevated temperatures. This reversal in behavior is explained by considering the effect of beta-stabilizer additions on the deformation mechanisms at room temperature and at elevated temperatures.     

Microstructural factors affecting superplastic properties in magnesium-based composites

Effect of microstructural factors on superplastic behavior in magnesium-based composites was reviewed in order to obtain insights on ways to enhance the superplastic properties, such as highstrain-rate superplasticity, low-temperature superplasticity, and high ductility. The review shows that the reduction in grain size of the matrix directly increases the strain rate and/or decreases the temperature for optimum superplastic flow. The effect of reinforcement addition is shown to reduce the superplastic elongation, but enhance the superplastic strain rate, presumably owing to grain size stability of composites at high temperatures. Ductility enhancement is not necessarily attained by refining initial grain size. It is suggested that it is necessary to disperse the reinforcement uniformly in order to obtain higher ductility.     

超塑性材料现状及新型超塑性低中碳合金钢研发

 在分析超塑性金属材料现状及发展趋势的基础上,对低中碳钢、高碳钢和双相不锈钢、奥氏体钢等钢铁材料的超塑性研究进行了归纳分析,提出了低成本量大面广低中碳合金钢将成为超塑性材料研发的一个重要方向。研究结果表明,通过科学合金化设计、精细组织调控和初步超塑性行为研究,可以获得在10－2/s应变速率和750～850 ℃下具有1 000%超塑性的低成本超塑性低中碳合金钢。这种优异超塑性性能主要归因于形成超细晶组织的合金化设计与组织调控。该研究成果打破传统低中碳钢不具有超塑性的局面,实现了可工业化超塑性能的低中碳合金钢创新发展,将推动超塑性钢材在航空航天和交通运输等领域的广泛应用。