Microstructure and superplasticity of Mg–Al–Ca electromagnetic casting alloys after hot extrusion

Microstructure and superplastic properties of the plates extruded from the Ca containing Mg alloy (1 wt.% Ca–AZ31) billets fabricated by electromagnetic casting (EMC) without and with electromagnetic stirring (EMS) were examined. The linear intercept grain sizes of the extruded materials were 3.7 μm and 2.1 μm, respectively. The material extruded from the EMC + EMS billet exhibited good superplasticity at low temperatures as well as at high strain rates, including the tensile elongations of 370% at 1 × 10⁻³ s⁻¹, −523 K and 550% at 1 × 10⁻² s⁻¹, −673 K. These values largely exceeded those of the AZ31 alloys with the similar grain sizes. The superior superplasticity of the extruded EMC + EMS billet could be attributed to fine grains and high grain stability at elevated temperatures by the presence of finely dispersed particles of thermally stable (Al,Mg)₂Ca phase. The constitutive equations were developed for describing the high-temperature deformation behavior of the fine-grained 1 wt.% Ca–AZ31 alloys with different grain sizes in wide range of temperature and strain rate.     

Forging of Mg–3Al–1Zn–1Ca alloy prepared by high-frequency electromagnetic casting

The 1 wt.%Ca–AZ31 alloy produced by electromagnetic casting (EMC) in presence of electromagnetic stirring (EMS) was extruded and then subjected to the closed-die forging to make a pulley for automobile application. Effective dynamic recrystallization (DRX) took place during the forging process, leading to formation of fully recrystallized grains with the average size of 3–4 μm. High-forging ability and high degree of grain refinement achieved during the forging were attributed to the novel microstructure of the cast composed of small and equiaxed grains with the average size of 50 μm and thin layer (Al, Mg)₂ Ca phase at grain boundaries, which would provide more nucleation sites and a faster rate of recrystallization during deformation by forging as compared to that of the conventionally processed cast composed of large size grains and thick layer (Al, Mg)₂ Ca phase. The forged pulley exhibited the ultimate tensile strength of 273–286 MPa with tensile elongations of 30%. The present result demonstrates a possibility that EMC + EMS techniques can be used in producing magnesium feed stocks with high-forging ability.     

Dynamic recrystallization during high temperature deformation of magnesium

As a consequence of the high critical stresses required for the activation of non-basal slip systems, dynamic recrystallization plays a vital role in the deformation of magnesium, particularly at a deformation temperature of 200 °C, where a transition from brittle to ductile behavior is observed. Uniaxial compression tests were performed on an extruded commercial magnesium alloy AZ31 at different temperatures and strain rates to examine the influence of deformation conditions on the dynamic recrystallization (DRX) behavior and texture evolution. Furthermore, the role of the starting texture in the development of the final DRX grain size was investigated. The recrystallized grain size, measured at large strains (  −1.4) seemed to be more dependent on the deformation conditions than on the starting texture. In contrast to pure magnesium, AZ31 does not undergo grain growth at elevated deformation temperatures, i.e. 400 °C, even at a low strain rate of 10⁻⁴ s⁻¹. Certain deformation conditions gave rise to a desired fully recrystallized microstructure with an average grain size of 18 μm and an almost random crystallographic texture. For samples deformed at 200 °C/10⁻² s⁻¹, optical microscopy revealed DRX inside of deformation twins, which was further investigated by EBSD.     

Microstructure and mechanical properties of Mg–Zn–Ca alloy processed by equal channel angular pressing

An ultrafine-grained (UFG) Mg–5.12 wt.% Zn–0.32 wt.% Ca alloy with an average grain size of 0.7 μm was produced by subjecting the as-extruded alloy to equal channel angular pressing (ECAP) for 4 passes at 250 °C. The fine secondary phase restricted the dynamic recrystallized (DRXed) grain growth during the ECAP processing, resulting in a remarkable grain refinement. A new texture was formed in the ECAPed Mg alloy with the {0 0 0 2} plane inclined at an angle of 58° relative to the extrusion direction. The yield stress (YS) was decreased in the as-ECAPed alloy with finer grains, indicating that the texture softening effect was dominant over the strengthening from grain refinement. The ductility of the as-ECAPed alloy was increased to 18.2%. The grain refinement caused an obvious decrease in work hardening rate in the as-ECAPed alloy during tensile deformation at room temperature.     

Quantitative study of grain refinement in Al–Mg alloy processed by equal channel angular pressing at cryogenic temperature

Strain induced grain refinement of an Al–1 wt.% Mg alloy processed by equal channel angular pressing (ECAP) at cryogenic temperature is investigated quantitatively. The results show that both mean grain and subgrain sizes are reduced gradually with increasing ECAP pass. ECAP at cryogenic temperature increases the rate of grain refinement by promoting the fraction of high angle grain boundaries (HAGBs) and misorientation at each pass. The fraction of HAGBs and the misorientation of Al–1 wt.% Mg alloy during ECAP at cryogenic temperature increase continuously as a function of equivalent strain. Both {110} and {111} twins at ultrafine-grained size are observed firstly in Al–Mg alloy during ECAP. The analysis of grain boundaries and misorientation gradients demonstrates the grain refinement mechanism of continuous dynamic recrystallization.     

Superplastic behavior of a fine-grained ZK60 magnesium alloy processed by high-ratio differential speed rolling

Grain size of the ZK60 alloy was effectively reduced to 12 μm through high-ratio differential speed rolling (HRDSR) for a thickness reduction of 70% in a single pass. Due to the strengthening effects of grain boundaries and particles, the HRDSR processed ZK60 exhibited a high tensile strength of 340 MPa. Low temperature superplasticity was attained at 473–493 K at low strain rates (5 × 10⁻⁴ s⁻¹) and high strain rate superplasticity was attained at 523–553 K at high strain rates (10⁻² s⁻¹). The optimum superplastic temperature was found to be 553 K where a maximum tensile elongation of 1000% was obtained at 1 × 10⁻³ s⁻¹. The deformation behavior of the HRDSR processed ZK60 at elevated temperatures could be depicted by considering contribution of grain boundary sliding and slip creep to total plastic flow. Difference in superplastic deformation behavior between the HRDSR processed and equal channel angular press processed ZK60 alloys was examined and discussed.     

Effect of welding speed on microstructural and mechanical properties of friction stir welded Inconel 600

In order to evaluate the properties of a friction stir welded Ni base alloy, Inconel 600 (single phase type) was selected. Sound friction stir welds without weld defect were obtained at 150 and 200 mm/min in welding speed, however, a groove like defect occurred at 250 mm/min. The electron back scattered diffraction (EBSD) method was used to analyze the grain boundary character distribution. As a result, dynamic recrystallization was observed at all conditions, and the grain refinement was achieved in the stir zone, and it was gradually accelerated from 19 μm in average grain size of the base material to 3.4 μm in the stir zone with increasing the welding speed. It also has an effect on the mechanical properties so that friction stir welded zone showed 20% higher microhardness and 10% higher tensile strength than those of base material.     

Achieving superplasticity at high strain rates using equal channel angular pressing

Abstract

Equal channel angular pressing (ECAP) is a processing procedure in which a sample is pressed through a die containing a channel bent into an L shaped configuration. This procedure introduces a high strain into the sample without any change in the cross-sectional area and it may be used to attain an ultrafine grain size with dimensions lying typically within the submicrometer range. This paper describes a series of experiments where ECAP was applied to a commercial Al–Mg–Li–Zr alloy having an initial grain size of ～400 µm. The results demonstrate a refinement in the grain size of this alloy to a size of ～1 µm and it is shown that these small grains are stable up to temperatures >600 K because of the presence of β′-Al₃Zr particles. The stability of these ultrafine grains at elevated temperatures provides an opportunity to achieve superplastic ductilities in this alloy at very high strain rates: for example, the measured elongations to failure under optimum pressing conditions exceed 1000% at a strain rate of 10^-1 s^-1 when testing at temperatures above 600 K.     

Effects of grain size on cyclic plasticity and fatigue crack initiation in nickel

Fatigue experiments were conducted on polycrystalline nickel of two grain sizes, 24 and 290 μm, to evaluate the effects of grain size on cyclic plasticity and fatigue crack initiation. Specimens were cycled at room temperature at plastic strain amplitudes ranging from 2.5×10⁻⁵ to 2.5×10⁻³. Analyses of the cyclic stress–strain response and evolution of hysteresis loop shape indicate that the back stress component of the cyclic stress is significantly affected by grain size and plastic strain amplitude, whereas these parameters have little effect on friction stress. A nonlinear kinematic hardening framework was used to study the evolution of back stress parameters with cumulative plastic strain. These are related to substructural evolution features. In particular, long range back stress components are related to persistent slip bands. The difference in cyclic plasticity behavior between the two grain sizes is related to the effect of grain size on persistent slip band (PSB) morphology, and the effect this has on long range back stress. Fine grain specimens had a much longer fatigue life, especially at low plastic strain amplitude, as a result of the influence of grain size on fatigue crack initiation characteristics. At low plastic strain amplitude (2.5×10⁻⁴), coarse grain specimens initiated cracks where PSBs impinged on grain boundaries. Fine grain specimens formed cracks along PSBs. At high plastic strain amplitude (2.5×10⁻³), both grain sizes initiated cracks at grain boundaries.     

Structural and electrical characterization of AgInS<Subscript>2</Subscript> thin films grown by single-source thermal evaporation method

Structural and electrical properties of AgInS₂ (AIS) thin films grown by single-source thermal evaporation method were studied. The X-ray diffraction spectra indicated that the AIS single phase was successfully grown by annealing above 400∘C in air. The grain size of the AIS crystals was above 2.5 μm from the surface photograph. Furthermore, the AIS grain sizes became large with increasing the annealing temperatures. All the samples indicated n-type conduction by the Van der Pauw technique. The carrier concentrations and the resistivities of the AIS films at room temperature were in the range of 10¹⁹–10²² cm⁻³ and 10⁻¹–10⁻³ Ωcm, respectively. Therefore the mobilities increased from 0.6 to 6.0 cm²/Vs with increasing the grain sizes.     

Effect of thermomechanical treatments on microstructure and properties of Cu-base leadframe alloy

The effect of thermomechanical treatments (TMT) on the microstructuresand properties of Cu-1.5Ni-0.3Si-0.03P-0.05Mg leadframe alloy wasinvestigated. The Cu-base leadframe alloy was received as hot rolledplates with 8 mm thickness. The hot rolled plates were solutiontreated at 700°C or 800°C for 1 hour, and coldrolled with 40–85% reduction, then followed by aging treatment at450°C. The leadframe alloy solution treated at 800°Cshowed larger grain size of 15 m comparing with the grain size of10 m in leadframe alloy solution treated at 700°C. Theleadframe alloy with smaller grain size of 10 m showed highertensile strength and lower electrical resistivity than that withlarger grain size of 15 m. The dislocation density increased withincreasing reduction ratio of cold rolling from 40% to 85% andresulted in finer Ni₂Si precipitates. Tensile strength increasedand electrical resistivity decreased with increasing reduction ratioof cold rolling due to the formation of finer Ni₂Si precipitates.Two types of thermomechanical treatments were performed to enhance theproperties of leadframe alloy. One type of thermomechanical treatmentis to refine the grain size through the overaging, cold rollingfollowed by recrystallization. The recrystallization process improvedthe tensile strength to 540 MPa and elongation to 15% by reducing thegrain size to 5 m. The other type of thermomechanical treatmentis to refine the precipitate size by two-step aging process. Thetwo-step aging process increased the tensile strength to 640 MPa andreduced the electrical resistivity to1.475 × 10^–8 m by reducing the size of Ni₂Si precipitates to 4 nm.     

Effects of nitrogen on microstructural evolution of biomedical Co–Cr–W alloys during hot deformation and subsequent cooling

The present study investigated how nitrogen affected the high-temperature deformation and microstructural evolution of biomedical Ni-free Co–Cr–W alloys during hot deformation. Hot compression tests of undoped and N-doped Co–28Cr–9W–1Si–0.05C (mass%) alloys were performed at deformation temperatures ranging from 1323 to 1473 K at strain rates of 10⁻³ to 10 s⁻¹. The microstructures, which were subjected to a true strain of 0.92 (60% in compression), were characterized using electron backscatter diffraction (EBSD) analysis and transmission electron microscopy (TEM). Dynamic recrystallization (DRX) was found to occur in both alloys during hot deformation. The grain size (d) decreased considerably with an increase in the Zener–Hollomon (Z) parameter. Although adding nitrogen to the alloys barely affected dynamic-recrystallization-induced grain refinement, it increased the magnitude of the flow stress and delayed static recrystallization during post-deformation cooling. Consequently, the N-doped alloy contained bulk nanostructures whose average grain size was 0.9 μm.     

Creep of magnesium strengthened with high volume fractions of yttria dispersoids

Creep experiments were performed on dispersion-strengthened-cast magnesium (DSC-Mg), consisting of unalloyed magnesium with 1 μm grain size containing 30 vol.% of 0.33 μm yttria particles. Strain rates were measured for temperatures between 573 and 723 K at compressive stresses between 7 and 125 MPa. DSC-Mg exhibits outstanding creep strength as compared with other magnesium materials, but is less creep resistant than comparable DSC-Al and other dispersion-strengthened aluminum materials. Two separate creep regimes were observed in DSC-Mg, at low stresses (σ<30 MPa), both the apparent stress exponent (n_app≈2) and the apparent activation energy (Q_app≈48 kJ mol⁻¹) are low, while at high stresses (σ>34 MPa), these parameters are much higher (n_app=9–15 and Q_app=230–325 kJ mol⁻¹) and increase, respectively, with increasing temperature and stress. The low-stress regime can be explained by an existing model of grain-boundary sliding inhibited by dispersoids at grain-boundaries. The unexpectedly low activation energy (about half the activation energy of grain boundary diffusion in pure magnesium) is interpreted as interfacial diffusion at the Mg/Y₂O₃ interface. The high-stress regime can be described by dislocation creep with dispersion-strengthening from the interaction of the submicron particles with matrix dislocations. The origin of the threshold stress is discussed in the light of existing dislocation climb, detachment and pile-up models.     

Exceptional superplasticity in an AZ61 magnesium alloy processed by extrusion and ECAP

Experiments were conducted on a commercial AZ61 alloy to evaluate the potential for achieving an ultrafine grain size and superplastic ductilities through the use of the EX-ECAP two-step processing procedure of extrusion plus equal-channel angular pressing. The results show that EX-ECAP gives excellent grain refinement with grain sizes of 0.6 and 1.3 μm after pressing at 473 and 523 K, respectively. The alloy processed by EX-ECAP exhibits exceptional superplastic properties including a maximum elongation of 1320% after pressing through four passes when testing at 473 K with an initial strain rate of 3.3 × 10⁻⁴ s⁻¹. This result compares with an elongation of 70% achieved in the extruded condition without ECAP under similar testing conditions.     

Three-dimensional measurement of ice crystals in frozen dilute solution

A Micro-Slicer Image Processing System (MSIPS) has been applied to observe the ice crystal structures formed in frozen dilute solutions. Several characteristic parameters were also proposed to investigate the three-dimensional (3-D) morphology and distribution of ice crystals, based on their reconstructed images obtained by multi-slicing a frozen sample with the thickness of 5 μm. The values of characteristic parameters were determined for the sample images with the dimension of 530×700×1000 μm. The 3-D morphology of ice crystals was found to be a bundle of continuous or dendrite columns at any freezing condition. The equivalent diameter of ice crystals were in the range of 73–169 μm, and decreased exponentially with increasing freezing rate at the copper cooling plate temperature of −20 to −80 °C. At the T_cp −40 °C, the volumes of ice crystals were in the range of 4.6×10⁴ μm³ to 3.3×10⁷ μm³, and 36 ice columns were counted in the 3-D image.     

Possibility of grain refinement for superplasticity of a Mg-AI-Zn alloy by pre-deformation

For a commercial Mg-Al-Zn alloy sheet, tensile tests are carried out under various strains, strain rates and temperatures to investigate the possibility of grain refinement by dynamic recrystallization during pre-deformation. It is found from the microstructural observations that relatively fine grains of 10 m or so, in diameter are attained under the conditions of 250°C and 8.3 × 10^–4 s^–1. The specimen pre-strained under this condition also exhibits a fairly good superplasticity of total elongation beyond 300%.     

Processing of nanocrystalline 8 mol% yttria-stabilized zirconia by conventional, microwave-assisted and two-step sintering

Manufacturing of near full dense (>97%) 8 mol% yttria-stabilized zirconia (8YSZ) nanopowder (15–33 nm) compacts was manipulated using conventional sintering (CS), two-step sintering (TSS) and microwave-assisted sintering methods. Microwave firing was performed via two different heating rates, i.e. 5 and 50 °C min⁻¹. Although, the lower rate microwave sintering (LMS) was found to yield the higher densities at lower temperatures, this regime ultimately did not provide higher final densities compared to the other methods. The higher rate microwave sintering (HMS) on the other hand managed to suppress the accelerated grain growth and resulted to a finer microstructure (0.9 μm) than LMS (2.35 μm) and CS (2.14 μm). In spite of the great capability of TSS method in fabricating the specimens with ultra-fine grains (0.29 μm), microstructural inhomogeneity and the long total sintering time (>20 h) in comparison with HMS (29 min) set restrictions on the application of TSS method. Based on the effect of grain size on the mechanical properties of ceramics, the specimens produced by TSS exhibited higher fracture toughness (3.16 ± 0.06 MPa m^1/2) than those obtained from CS (1.61 ± 0.07 MPa m^1/2) and LMS (1.9 ± 0.09 MPa m^1/2), due to their finer grain size. The proximity in the fracture toughness values of TSS and HMS (3.17 ± 0.10 MPa m^1/2) samples stems from the higher microstructural homogeneity caused by HMS, while having a larger grain size.     

Solid–liquid interfacial energy of camphene

The Gibbs–Thomson coefficient and the solid–liquid interfacial energy for camphene have been measured to be (8.58±0.96)×10⁻⁸ K m and (4.43±0.49)×10⁻³ J m⁻², respectively, by a direct method. The grain boundary energy of camphene has also been calculated to be (8.36±0.92)×10⁻³ J m⁻² from the observed grain boundary groove shapes.     

Effect of grain size on high-cycle fatigue properties in alpha-type titanium alloy at cryogenic temperatures

High-cycle fatigue properties were investigated at 4, 77 and 293 K in Ti-5%Al-2.5%Sn ELI alloy which was used for liquid hydrogen turbo-pumps of Japanese-built launch vehicles. Mean grain size of specimens was controlled to be about 30 or 80 μm. In the specimens with a grain size of 30 μm, fatigue strengths at 10⁶ cycles at 4 and 77 K are 1.6 and 1.5 times higher than that at 293 K, respectively. On the other hand, in the specimen with a grain size of 80 μm, fatigue strengths at 10⁶ cycles at 4 and 77 K get lower to the same level as that at 293 K. Thus, it is concluded that refinement of α grains is one of important factors to obtain the good high-cycle fatigue properties for Ti-5%Al-2.5%Sn ELI alloy at cryogenic temperature.     

Influence of rolling temperature on static recrystallization behavior of AZ31 magnesium alloy

Poor formability of rolled magnesium (Mg) alloys extremely restricts applications in form of sheets originating from formation of strong basal texture. Recently, we found that increasing rolling temperature from 723 to 798 K for a AZ31 Mg alloy can significantly improve stretch formability due to remarkable texture weakening after annealing. In this study, static recrystallization behaviors of AZ31 alloy sheets rolled at 723 and 798 K were investigated by electron backscattered diffraction analyses at different annealing stages in order to understand the origin of high temperature rolling on texture weakening. For both sheets, similar deformation microstructures with approximately the same types and fractions of twins exist in the as-rolled condition and recrystallized grains are mainly formed at pre-existing grain boundaries due to discontinuous recrystallization during subsequent annealing. However, only the basal texture of the latter remarkably weakens due to the formation of new recrystallized grains with well-dispersed orientations. Non-basal slips enhanced during high temperature rolling at 798 K are most likely responsible for the texture randomization as a result of rotations of recrystallization nuclei.