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.     

Achieving enhanced ductility in a dilute magnesium alloy through severe plastic deformation

Experiments were conducted to evaluate the utility of a new processing procedure developed for Mg-based alloys in which samples are subjected to a two-step processing route of extrusion followed by equal-channel angular pressing (designated as EX-ECAP). The experiments were conducted using a Mg-0.6 wt pct Zr alloy and, for comparison purposes, samples of pure Mg. It is shown that the potential for successfully using ECAP increases in both materials when adopting the EX-ECAP procedure. For the Mg-Zr alloy, the use of EX-ECAP produces a grain size of ∼1.4 μm when the pressing is undertaken at 573 K. By contrast, using EX-ECAP with pure Mg at 573 K produces a grain size of ∼26 μm. Tensile testing of the Mg-Zr alloy at 523 and 573 K after processing by EX-ECAP revealed the occurrence of significantly enhanced ductilities with maximum elongations of ∼300 to 400 pct.     

Effects of composition and microstructure on fatigue of γ/γ′-δ type eutectic alloys

Room temperature tension-tension fatigue tests were performed on two lamellar γ/γ′-δ alloys, one with 0 pct Cr and one with 6 pct Cr. The 6 pct Cr alloy was solidified at 3 cmJh while the 0 pct Cr alloy was solidified at 3 cm/h and 5.7 cm/h. Fatigue testing was done on both alloys in the as-directionally solidified condition and on the 0 pct Cr alloy after heat treatment. Increasing the growth speed of the 0 pct Cr alloy increased the fatigue life of the material at stresses above the 10⁷ cycle fatigue limit. Partial solution treating and aging of the 0 pct Cr alloy,R = 3 cm/h, increased the fatigue life relative to the as-directionally solidified material at high stresses, to the same extent as increasing the growth speed. Full solution treatment and aging of the 0 pct Cr alloy,R = 5.7 cm/ h, caused a reduction in the fatigue life relative to the as-directionally solidified material. Fatigue cracking tended to be faceted in the 6 pct Cr alloy as opposed to the more ductile failure of the 0 pct Cr alloy. Microstructural perfection, grain size and shape, interlamellar spacing, longitudinal cracking, and longitudinal and transverse ductility all are believed to have influenced the fatigue resistance of the alloys.     

Influence of pressing speed on microstructural development in equal-channel angular pressing

The influence of pressing speed in equal-channel angular (ECA) pressing was investigated using samples of pure Al and an Al-1 pct Mg alloy and a range of pressing speeds from ∼10⁻² to ∼10 mm s⁻¹. The results show that the speed of pressing has no significant influence on the equilibrium grain size, at least over the range used in these experiments. Thus, the equilibrium grain sizes were ∼1.2 μm for pure Al and ∼0.5 μm for the Al-1 pct Mg alloy for all pressing conditions. However, it is shown that the nature of the microstructure is dependent on the pressing speed, because recovery occurs more easily at the slower speeds, so that the microstructure is then more equilibrated. There is also indirect evidence for the advent of frictional effects when the cross-sectional dimensions of the samples are at or below ∼5 mm.     

Effect of B on the microstructure and mechanical properties of mechanically milled TiAl alloys

The present study is concerned with γ-(Ti₅₂Al₄₈)_100−x B _x (x=0, 0.5, 2, 5) alloys produced by mechanical milling/vacuum hot pressing (VHPing) using melt-extracted powders. Microstructure of the as-vacuum hot pressed (VHPed) alloys exhibits a duplex equiaxed microstructure of α₂ and γ with a mean grain size of 200 nm. Besides α₂ and γ phases, binary and 0.5 pct B alloys contain Ti₂AlN and Al₂O₃ phases located along the grain boundaries and show appreciable coarsening in grain and dispersoid sizes during annealing treatment at 1300 °C for 5 hours. On the other hand, 2 pct B and 5 pct B alloys contain fine boride particles within the γ grains and show minimal coarsening during annealing. Room-temperature compressing tests of the as-VHPed alloys show low ductility, but very high yield strength >2100 MPa. After annealing treatment, mechanically milled alloys show much higher yield strength than conventional powder metallurgy and ingot metallurgy processed alloys, with equivalent ductility to ingot metallurgy processed alloys. The 5 pct B alloy with the smallest grain size shows higher yield strength than binary alloy up to the test temperature of 700 °C. At 850 °C, 5 pct B alloy shows much lower strength than the binary alloy, indicating that the deformation of fine 5 pct B alloy is dominated by the grain boundary sliding mechanism. 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.     

Texture evolution and mechanical anisotropy in dual-phase Ti<Subscript>3</Subscript>Al-based alloy loaded at 700 °C to 1000 °C

The super α ₂ Ti₃Al-based alloy with a fine grain size of ∼2.2 μm exhibits superplastic elongations over 1000 pct at 920 °C to 1000 °C, 600 pct at 900 °C, 330 pct at 850 °C, and 140 pct at 750 °C. Mechanical anisotropy is observed in this alloy, and relatively lower flow stresses and higher tensile elongations are obtained in the 45 deg specimen loaded at 25 °C to 960 °C. The texture characteristics appear to impose significant influence on the mechanical anisotropy at temperatures below 900 °C (under the dislocation creep condition), and the {111}〈2 〉 and {0001} basal textures evolve in the β and α ₂ phases after tensile straining. At loading temperatures higher than 900 °C (under the superplastic flow condition), the anisotropy effect is less pronounced and the grain orientation distribution becomes basically random in nature. Rationalizations for the mechanical anisotropy in terms of the Schmid factor calculations for the major and minor texture components in the β and α ₂ phases provide consistent explanations for the deformation behavior at lower temperatures as well as the initial straining stage at higher temperatures.     

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.     

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.     

Precipitation of austenite particles at grain boundaries during aging of Fe-Mn-Ni steel

Precipitation of austenite particles at grain and lath boundaries after aging treatment of a Fe-8Mn-7Ni alloy was investigated by selected area electron diffraction (SAD), X-ray energy dispersive spectrometry (EDS) in a scanning transmission electron microscope (STEM), and high-resolution (HRTEM) analysis. High spatial-resolution (2 to 5 nm) EDS analysis revealed no significant segregation of alloying elements at grain boundaries but the precipitation of very fine particles of Mn- and Ni-rich phase. Detailed EDS, SAD, and HRTEM analyses all confirmed that these particles are austenite phase, which have a Kurdjumov-Sachs (K-S) orientation relationship with one of the adjacent grain. The concentration of Mn and Ni in austenite, measured by EDS, varied from ∼15 pct to a maximum of ∼30 pct. Low-voltage scanning electron microscopy (SEM) fractographs also revealed the presence of very fine, second-phase precipitates on the fracture surface of the embrittled alloys.     

Grain refinement and superplasticity in a magnesium alloy processed by equal-channel angular pressing

The extrusion/equal channel angular pressing (EX-ECAP) processing procedure, in which magnesium-based alloys are subjected to extrusion followed by ECAP, was applied to a Mg-7.5 pct Al-0.2 pct Zr alloy prepared by casting. Microstructural inspection showed the EX-ECAP process was effective in reducing the grain size from ∼21 μm after extrusion to an as-pressed grain size of ∼0.8 μm. It is shown through static annealing that these ultrafine grains are reasonably stable up to 473 K, but grain growth occurs at higher temperatures. Tensile specimens were cut from the billets prepared by EX-ECAP and testing showed these specimens exhibited superplasticity at relatively low temperatures with maximum elongations up to >700 pct. By processing through EX-ECAP to a higher imposed strain and thereby increasing the area fraction of high-angle boundaries, it is demonstrated that there is a potential for achieving high-strain-rate superplasticity. This article is based on a presentation made at the Symposium entitled “Phase Transformations and Deformation in Magnesium Alloys,” which occurred during the Spring TMS meeting, March 14–18, 2004, in Charlotte, NC, under the auspices of the ASM-MSCTS Phase Transformations Committee.     

A metallographic study of porosity and fracture behavior in relation to the tensile properties in 319.2 end chill castings

A metallographic study of the porosity and fracture behavior in unidirectionally solidified end chill castings of 319.2 aluminum alloy (Al-6.2 pct Si-3.8 pct Cu-0.5 pct Fe-0.14 pct Mn-0.06 pct Mg-0.073 pct Ti) was carried out using optical microscopy and scanning electron microscopy (SEM) to determine their relationship with the tensile properties. The parameters varied in the production of these castings were the hydrogen (∼0.1 and ∼0.37 mL/100 g Al), modifier (0 and 300 ppm Sr), and grain refiner (0 and 0.02 wt pct Ti) concentrations, as well as the solidification time, which increased with increasing distance from the end chill bottom of the casting, giving dendrite arm spacings (DASs) ranging from ∼15 to ∼95 /im. Image analysis and energy dispersive X-ray (EDX) analysis were employed for quantification of porosity/microstructural constituents and fracture surface analysis (phase identification), respectively. The results showed that the local solidification time(viz. DAS) significantly influences the ductility at low hydrogen levels; at higher levels, however, hydro-gen has a more pronounced effect (porosity related) on the drop in ductility. Porosity is mainly observed in the form of elongated pores along the grain boundaries, with Sr increasing the porosity volume percent and grain refining increasing the probability for pore branching. The beneficial effect of Sr modification, however, improves the alloy ductility. Fracture of the Si, β-Al₅FeSi, α- Al₁₅(Fe,Mn)₃Si₂, and Al₂Cu phases takes place within the phase particles rather than at the particle/Al matrix interface. Sensitivity of tensile properties to DAS allows for the use of the latter as an indicator of the expected properties of the alloy.     

The effects of stress level and grain size on the ambient temperature creep deformation behavior of an alpha Ti-1.6 wt pct V alloy

Ambient (room) temperature studies have been carried out on an α-Ti-1.6 wt pct V alloy to determine the effects of stress level and grain size on ambient temperature creep behavior. Creep tests were performed at five different stress levels ranging from 75 to 95 pct of the yield stress value on specimens with an average grain size of 226 μm. It has been found that the alloy exhibits appreciable creep at stress levels far below the yield stress, with creep occurring at values as low as 75 pct of the yield stress. The extent of creep strain was found to decrease with a decrease in stress level. Creep tests were also performed on this alloy with different grain sizes ranging from 38 to 226 μm at a stress level of 90 pct of the yield stress. It was seen that the extent of creep strain decreased with a decrease in grain size. Fine slip and time-dependent twinning were found to be the creep deformation mechanisms. Based on the results of this investigation and earlier studies, it is suggested that time-dependent twinning is a major creep deformation mechanism in α-titanium alloys that contain small amounts of alloying elements. The time-dependent twinning phenomenon has been attributed to the diffusion of oxygen away from the twin-matrix interface, permitting the growth of twins.     

A fine γ′+α cellular structure in Fe-37.3 wt pct Ni-3.6 wt pct Al-3.3 wt pct Ti-0.2 wt pct C and its influence on high-temperature tensile properties

Fe-37.3 wt pct Ni-3.6 wt pct Al-3.3 wt pct Ti-0.2 wt pct C alloy, which reveals an excellent combination of high strength and good elongation endowed by formation of homogeneously dispersed fine γ′ precipitates in the matrix during aging at 823 K, has been investigated by means of transmission electron and optical microscopies, electron diffractions, and tensile tests. The influence of unique γ′+α cellular products on the mechanical properties has also been studied. Because of low elastic mismatch between the austenitic γ matrix and isomorphic γ′ precipitate phases, the homogeneously distributed precipitate particles, which formed at the early stage of aging, were observed to persist even after long-term aging. After very lengthy aging, the fine γ′ phase particles were changed to coarser γ′ lamellae at the grain boundary reaction front, which were alternately arranged with fine α lamellae that were estimated to have been transformed from the austenite-stabilizing-solute(Ni, C)-depleted γ lamellae. The fine duplex γ′+α cellular product did not affect deleteriously the room-temperature tensile properties of the alloy. However, the cellular structure was observed to cause the grain boundary embrittlement of the aged alloy at elevated temperatures higher than 681 K.     

On the behavior of microstructures with multiple length scales

The current study aims to provide fundamental insight into the behavior of microstructures containing grain sizes that span multiple length scales. A commercial 5083 Al alloy was selected as the material of interest to facilitate comparison with recently published data. The materials studied here were prepared via the thermal consolidation of powders that were cryomilled for different times (i.e., 0, 2, 4, and 8 hours). Following consolidation, the resultant microstructure was characterized by an equiaxed grain morphology with a size distribution centered around 200∼300 nm. Dispersed among the 200- to 300-nm grains were coarse-grained regions or ligaments with a grain size ranging from 600 nm to 2 μm. The occurrence of coarse-grained regions is rationalized on the basis of recrystallization or subgrain coarsening, whereas the occurrence of equiaxed fine regions is proposed to be a result of continuous grain growth. Two types of microstructures were selected for study, containing coarse-grained volumes of approximately 28 pct and 43 pct that corresponded to an ultimate tensile strength (UTS) of 566 MPa and 535 MPa, and a fracture strain of 3.2 pct and 3.5 pct, respectively. The observed ductility and the relevant toughening mechanisms were discussed in light of the presence of multiple length scales.     

Effect of Solution Temperature on the Microstructure and Mechanical Properties of a Newly Developed Superalloy TMW-4M3

The influence of solution temperature on the microstructure and mechanical properties of TMW-4M3 superalloy has been investigated. Comparisons of mechanical properties have also been made between the heat-treated TMW-4M3 variants and the commercial U720Li. The key microstructural variables examined were grain size and the volume fraction and size of the strengthening γ′ precipitates that control the mechanical properties of these alloys. By increasing the solution temperature from 1373 K to 1393 K (1100 °C to 1120 °C), the volume fraction of primary gamma prime dropped from 16.9 pct to 14.5 pct, whereas the average grain size increased from 8.7 μm to 10.6 μm. Compared with an alloy with a smaller grain size, the alloy with a larger grain size exhibited superior resistances to creep and fatigue crack growth without the expense of reduced tensile strength and low-cycle fatigue resistance. This suggested that a higher solution temperature may benefit TMW-4M3 in terms of superior overall properties. The greater overall properties of TMW-4M3 variants than that of commercial U720Li were also demonstrated experimentally. The possible explanations for the improvement of mechanical properties were discussed.     

Effects of the amount of γ′ and oxide content on the secondary recrystallization temperature of nickel-base superalloys

The effects of the amount of γ′ and yttria (Y₂O₃) content on the secondary recrystallization (SRx) temperature of as-extruded material of the mechanically alloyed nickel-base superalloys based on a superalloy TMO-2 were investigated. It was observed that (1) the primarily recrystallized grain size of the as-extruded material decreased with increasing the γ′ and the yttria content in the material; (2) the SRx temperature decreased with decreasing the yttria content and with increasing the amount of theγ′ up to about 55 vol pct, while (3) the temperature increased for the material containing more than 65 vol pctγ′; and (4) the SRx temperatures of the material containing 75 vol pctγ′ phase with 1.1 wt pct yttria and 55 vol pctγ′ phase with no yttria were identical to theirγ′ solvus. From these results, the following conclusions are drawn: (1) dissolution of theγ′ particles is a necessary, but not a sufficient, condition for the occurrence of secondary recrystallization; (2) secondary recrystallization of a material with sufficiently smaller grain size occurs at a temperature higher than theγ′ solvus and the temperature at which the yttria particles lose their ability to prevent rapid growth of the primarily recrystallized grains; and (3) the SRx temperature of a material with larger grain size depends on grain size. Formerly Assistant Researcher with NRIM     

The effect of Sr and Fe additions on the microstructure and mechanical properties of a direct squeeze cast Al-7Si-0.3Mg alloy

This article describes the results of an investigation into the microstructure and mechanical properties of a gravity die cast and direct squeeze cast LM25 alloy (Al-7Si-0.3Mg-0.3Fe). The direct squeeze cast LM25 alloy has superior mechanical properties compared to the gravity die cast LM25 alloy, especially with regard to ductility, which is increased from ∼1.7 pct for the gravity die cast LM25 alloy to ∼8.0 pct for the direct squeeze cast LM25 alloy in the T6 heat-treated condition. This increase in ductility is due to (1) the removal of porosity, (2) a decrease in Si particle size, and (3) a refinement of the Fe-Si-aluminide particles. High cooling rates in direct squeeze casting result in quench modification of the Si particles, such that chemical modification with Sr or Na may not be required. In addition, direct squeeze casting is more tolerant of Fe impurities in the alloy, due to the formation of smaller Fe-Si-aluminide particles than those in gravity die cast material. The direct squeeze cast LM25+Fe alloy (Al-7Si-0.3Mg-1.0Fe) has a ductility of ∼6.5 pct, compared to that of ∼0.5 pct for the gravity die cast LM25 + Fe alloy in the T6 heat-treated condition. This increase in tolerance to Fe impurities can lead to a substantial reduction in manufacturing costs due to (1) reduced raw-material costs, (2) reduced die sticking, and (3) improved die life.     

Transition of dominant diffusion process during superplastic deformation in AZ61 magnesium alloys

The superplastic behavior of the AZ61 magnesium alloy sheet, processed by one-step hot extrusion and possessing medium grain sizes of ∼12 μm, has been investigated over the temperature range of 523 to 673 K. The highest superplastic elongation of 920 pct was obtained at 623 K and a deformation rate of 1×10⁻⁴ s⁻¹. In the lower and higher strain rate regimes, with apparent m values of ∼0.45 and ∼0.25, respectively, grain-boundary sliding (GBS) and dislocation creep appeared to dominate the deformation, consistent with the scanning electron microscopy (SEM) examination. The SEM examination also revealed that individual GBS started to operate from the very initial deformation stage in the strain rate range with m∼0.45, which was attributed to the relatively high fraction (88 pct) of high-angle boundaries. The analyses of the superplastic data over 523 to 673 K and 5×10⁻⁵ to 1×10⁻³ s⁻¹ revealed a true stress exponent of ∼2, and the activation energy was close to that for grain-boundary and lattice diffusion of magnesium at 523 to 573 K and 573 to 673 K, respectively. The transition temperature of activation energy is ∼573 K, which is attributed to the change in the dominant diffusion process from grain-boundary diffusion to lattice diffusion. It is demonstrated that the effective diffusion coefficient is a valid parameter to characterize the superplastic behavior and the dominant diffusion process.     

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.