Microstructural evolution during extrusion and ECAP of a spray-deposited Al–Zn–Mg–Cu–Sc–Zr alloy

The microstructural evolution of an Al–Zn–Mg–Cu–Sc–Zr alloy prepared by spray deposition via extrusion and equal-channel angular pressing (ECAP) was investigated in this study. Deformation route A for Al–11.5 wt% Zn–2 wt% Mg–1.5 wt% Cu–0.2 wt% Sc–0.15% Zr super-strength alloy was carried out at 573 K by ECAP. The microstructures of extruded and ECAP samples were investigated by means of Electron Backscatter Diffraction (EBSD), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). A large amount of dislocation tangles were formed inside grains during ECAP, which further evolved into sub-boundaries and high angle grain boundaries. Microstructure analyses showed that the grain size was refined to 800 nm after 8 passes ECAP from earlier 3.5 μm of sprayed and extruded alloy. A few finer MgZn₂ and Al₃(Sc,Zr) were dispersed uniformly after ECAP. The textures of 8 passes ECAPed sample were dominated by the strong Cu orientation and relatively weak S orientation.     

Microstructure and mechanical properties of ultrafine grain ZK60 alloy processed by equal channel angular pressing

The microstructure evolution and tensile properties of ZK60 magnesium alloy after equal channel angular pressing (ECAP) have been investigated. The results show that the two-step ECAP process is more effective in grain refinement than the single-step ECAP process due to the lower deformation temperature, a mean grain size of ~0.8 μm was obtained after two-step ECAP process at 513 K for four passes and 453 K for four passes. The EBSD examination reveals that ZK60 alloy after two-step ECAP process exhibits a more homogeneous grain size and misorientation distribution than single-step ECAP process. Both alloys after ECAP process present similar strong {0002} texture. The tensile strength of two-step ECAP alloy has also been improved compared with the single-step ECAP alloy. The strengthening effect was mainly ascribed to grain refinement.     

Thermophysical Properties of Aluminum 1060 Fabricated by Equal Channel Angular Pressing

Equal channel angular pressing (ECAP) has the advantage of enabling an ultrafine grain size. Aluminum 1060 is used as a power plant material because of its favorable electrical properties. However, the weak strength of aluminum limits its application. In this study, the thermal conductivity and electrical conductivity of Al 1060 made by ECAP was investigated. ECAP was conducted through the die having a channel angle of 90° and a corner angle of 20° at a temperature of 473 K with a strain rate of 2 mm · s⁻¹. The specimen was then processed with 1 to 8 passes by the route Bc method with 90° rotation. In the case of eight passes, the grain size was reduced to as small as 300 nm. As a result of the ECAP, the tensile strength was raised from 75 MPa to 134 MPa, while the electrical conductivity did not show a significant difference after eight passes. The thermal conductivity gradually decreased with ECAP passes, because of the decreased grain size by ECAP.     

Mechanical behaviour and texture of annealed AZ31 Mg alloy deformed by ECAP

Abstract

AZ31 Mg alloy samples were processed by equal channel angular pressing (ECAP) at 220°C for four passes. An average grain size of ～1·9 μm with reasonable homogeneity was obtained. The ECAP process imparted large plastic shear strains and strong deformation textures to the material. Subsequent annealing of the equal channel angular pressed samples produced interesting mechanical behaviours. While yield strength increased and ductility decreased immediately after undergoing ECAP, annealing at temperatures <250°C restored ductility significantly at a small decrease in of yield strength. Annealing at temperatures >250°C reduced yield strength without additional improvement in ductility. It is believed that the combination of stress relief via dislocation elimination, refined microstructure and the retention of a strong ECAP texture at low annealing temperatures enhance ductility. High temperature annealing breaks down the ECAP texture resulting in no further improvement in ductility. The results show that the mechanical properties of the alloy can be positively influenced by annealing after ECAP to achieve a combination of strength and ductility.     

Evolution of microstructure and texture in an ultrafine-grained Al6082 alloy during severe plastic deformation

The evolution of microstructure and texture in Al6082 precipitation-hardened alloy during equal-channel angular pressing (ECAP) was studied. It was found that although the dislocation density and the subgrain size saturated after 1 pass, the size of grains bounded by high angle boundaries reached its minimum value only after 4 passes. Furthermore, the grain orientation distribution changes between 4 and 8 passes, indicating the development of grain boundary structure even after the saturation of the parameters of the microstructure. As a result of this evolution, the initial texture of the commercial alloy was diminished after 8 passes and the grain orientation distribution became to be close to random case.     

Investigation of texture and mechanical properties of copper processed by new route of equal channel angular pressing

The evolution of crystallographic texture and the mechanical properties of copper subjected to severe plastic deformation (SPD) using equal channel angular pressing (ECAP) were investigated. Samples were subjected to ECAP under two different processing routes: B₆₀ and B_C. As the cross sections of the samples were circular, a new route with a rotation angle of 60° in the same direction between consecutive passes was introduced. The material exhibited texture development similar to the simple shear texture in both routes and the most significant changes in texture strength in both processing routes took place after the second pass. Microstructure of ECAP processed samples were investigated using electron backscatter diffraction (EBSD) analysis. Comparison of the EBSD data with optical micrograph of the initial sample confirmed that ECAP process has led to a significant decrease in grain size. Significant increases in hardness and tensile strength were observed after the first pass of ECAP. Variations of tensile strength as a function of the number of passes were related to the dislocation densities and the average boundary spacing.     

Grain boundary misorientation and positron annihilation characteristics in steel Eurofer processed by equal channel angular pressing

Electron back-scattered diffraction and positron annihilation lifetime measurements were performed on the ferritic–martensitic 9 %Cr Eurofer steel processed by equal channel angular pressing (ECAP) at 550 °C. The orientation imaging mapping images reveal ECAP-induced changes toward a more stable texture via rotation around 〈111〉 and 〈110〉 axes. These are accompanied by transformation of martensite into ferrite and a remarkable change in the bimodal distribution of grain misorientations with reduction of the fraction of high-angle grain boundaries. The positron annihilation measurements evidence the release of vacancies retained in the ECAP-processed material and their clustering into nanovoids in samples heat treated at T ≥ 500 °C. It is found that tensile strain applied at 600 °C can inhibit this void formation in the ECAP-deformed material for 1 and 2 passes, but not in the case of 4 passes. A model for accounting the results is proposed.     

Microstructure and strength of pure Cu with large grains processed by equal channel angular pressing

The pure Cu rods with an initial grain size of 410 μm were treated by using equal channel angular pressing (ECAP). The deformed microstructure and mechanical properties of ECAPed Cu samples were investigated. Special attention was paid on the refinement of grain size and local micromechanics of ECAPed Cu samples. The original coarse grains were refined to 320 μm after 4 passes. The final grains were composed of dislocation cells with a size of 500 nm–3 μm after 5–8 passes. The yield strength reached a saturation value of 368 MPa after 5 passes. The maps of microhardness distribution illustrated the inhomogeneity of local mechanical properties. The dislocation subdivision was the main deformation mode to refine the grain size, while twin fragmentation was restrained by dislocation slips for the reason of large initial grain size. Furthermore, the strengthening of ECAPed Cu was discussed.     

EBSD investigation of the microstructure and microtexture evolution of 1050 aluminum cross deformed from ECAP to plane strain compression

Electron backscattered diffraction (EBSD) was used to document the microstructure and texture developed due to cross deformation of commercial purity 1050 aluminum alloy. The materials are first deformed in equal channel angular pressing die (ECAP) to different number of passes; 1,4, 8, 12, and 16 passes, via route B_C and then deformed in plane strain compression (PSC) to two axial true plastic strain values of 0.5 and 1.0. Deformation path change was proven to be a very effective tool for manipulating the evolution of microstructure and microtexture. The study provides a documentation of the evolution of microstructure parameters namely cell size, misorientation angle, fraction of submicron grain size, and fraction of high angle grain boundaries. These microstructure parameters were investigated on two planes; the plane normal to the loading direction in PSC (RD–TD) and that plane normal to the transverse direction (RD–ND). These microstructure parameters are compared to those achieved due to the ECAP process only. The ideal rolling texture orientations are depicted and crystal orientation maps were generated. The spatial distribution of grains having these orientations is revealed through these maps. The fraction of the main texture components for a 10° spread around the specified orientations is experimentally calculated and a quantitative idea on the evolution of microtexture is also presented.     

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.     

Enhanced superplasticity of magnesium alloy AZ31 obtained through equal-channel angular pressing with back-pressure

Excellent superplastic elongations (in excess of 1,200%) were achieved in a commercial cast AZ31 alloy processed by low temperature equal-channel angular pressing (ECAP) with a back-pressure to produce a bimodal grain structure. In contrast, AZ31 alloy processed by ECAP at temperatures higher than 200 °C showed a reasonably uniform grain structure and relatively low ductility. It is suggested that a bimodal grain structure is advantageous because the larger grains contribute to strain hardening thus delaying the onset of necking, while grain boundary sliding associated with small grains provides a stabilizing effect due to enhanced strain rate sensitivity.     

Microstructure evolution and hardness variation during annealing of equal channel angular pressed ultra-fine grained nickel subjected to 12 passes

The microstructure, thermal stability and hardness of ultra-fine grained (UFG) Ni produced by 12 passes of equal channel angular pressing (ECAP) through the route Bc were studied. Comparing the microstructure and hardness of the as-ECAPed samples with the published data on UFG Ni obtained after 8 passes of ECAP through the route Bc reveals a smaller average grain size (230 nm in the present case compared with 270 nm in 8-pass Ni), significantly lower dislocation density (1.08 × 10¹⁴ m⁻² compared with 9 × 10¹⁴ m⁻² in 8-pass Ni) and lower hardness (2 GPa compared with 2.45 GPa for 8-pass Ni). Study of the thermal stability of the 12-pass UFG Ni revealed that recovery is dominant in the temperature range 150–250°C and recrystallisation occurred at temperatures >250 °C. The UFG microstructure is relatively stable up to about 400 °C. Due to the lower dislocation density and consequently a lower stored energy, the recrystallisation of 12-pass ECAP Ni occurred at a higher temperature (~250 °C) compared with the 8-pass Ni (~200 °C). In the 12-pass Nickel, hardness variation shows that its dependence on grain size is inversely linear rather than the common grain size^−0.5 dependence.     

DSC and TEM analysis of lattice defects governing the mechanical properties of an ECAP-processed magnesium alloy

The mechanical properties of the Mg alloy AM60 can be improved significantly by severe plastic deformation (SPD). The lower the temperature (down to 150 °C) of equal channel angular pressing (ECAP) the higher is the resulting strength (up to 310 MPa) which can be ascribed to the concomitant decrease of grain size (down to 1 μm). After ECAP-processing at temperatures 150–210 °C the ductility remains at about the same high level (∼15%) as in the initial material. This is explained with the presence of Al₁₂Mg₁₇ precipitates with a size of about 500 nm, which decrease the remaining concentration of Al in the solid solution of the matrix. Differential scanning calorimetry (DSC) revealed four peaks during heating runs. The most remarkable peak occurs at 390 °C in the initial sample, and at 360 °C in the material ECAPed at 150 °C. Transmission electron microscopy (TEM) analyses showed that this peak can be associated with the dissolution of the Al₁₂Mg₁₇ precipitates as well as with the annealing of dislocations and possibly vacancy clusters, and that ECAP has the potential to induce a shift of a phase boundary to lower temperatures because of ECAP induced lattice defects.     

Twist-channel angular pressing: effect of the strain path on grain refinement and mechanical properties of copper

Substructural characteristics of Cu (99.97%) were examined after the Twist channel angular pressing (TCAP) process carried out at ambient temperature. Grain refinement efficiency and resulting thermal stability were evaluated after three passes with respect to utilization of various strain paths. Results were obtained using light microscopy and X-ray diffraction methods; Mechanical properties of extruded materials were also tested. Thermal stability was studied after application of three annealing cycles. Based on the findings, Bc route is the most efficient strain path with respect to the grain refinement; higher speed of extrusion (10 mm/s) corresponds with suppression of the static recrystallization. Measured strength, obtained after three passes (route A), achieved values around 440 MPa homogeneously along the cross section of the extruded material. Homogeneity of deformation was also confirmed by micro-hardness tests. The grain size, determined after three passes, averaged out 1.2 μm. Application of TCAP (three passes) brought markedly homogeneous deformation throughout the processed sample in comparison with classical ECAP process.     

Texture simulation of aluminum rod during equal channel angular pressing

A general procedure for texture simulation in multi-pass equal channel angular pressing (ECAP) with capability of applying different processing routes is proposed. The program inputs are the initial texture and the loading condition and the output is texture after deformation. Deformation texture in ECAP of aluminum rod was predicted based on simple shear model for deformation and Visco plastic self consistent model for texture simulation. The simulation was done for two consecutive passes of ECAP and the results were compared with experimental texture measurements. The initial texture of the sample before ECAP was found to play a key role in formation of the final texture and a good agreement between the simulated and the experimental texture was obtained.     

Achieving superplastic properties in a Pb–Sn eutectic alloy processed by equal-channel angular pressing

Experiments were conducted on a Pb-62% Sn eutectic alloy containing 160 ppm of Sb. The alloy was processed by equal-channel angular pressing (ECAP) through 1 to 5 passes at room temperature and then tested in tension at a temperature of 423 K using initial strain rates from 1.0 × 10⁻⁴ to 1.0 × 10⁻¹ s⁻¹. Excellent superplastic elongations were achieved at intermediate strain rates with a maximum elongation to failure of 2,665%. It is shown that, for processing through similar numbers of ECAP passes, these elongations are higher than in an earlier investigation using a Pb-62% Sn alloy of higher purity. The results are presented pictorially in the form of a deformation mechanism map by plotting normalized grain size against normalized stress at a temperature of 423 K.     

Microstructural evolution in high purity aluminum processed by ECAP

High purity (99.99%) aluminum was processed by equal-channel angular pressing (ECAP) through 1–12 passes and examined using orientation imaging microscopy. The results reveal two distinct processing regimes: from 1 to 4 passes the microstructure evolves from elongated subgrains to an essentially equiaxed array of ultrafine grains and from 4 to 12 passes there is no measurable change in the average grain size and grain aspect ratio. The boundary misorientation angle and the fraction of high-angle boundaries increase rapidly up to 4 passes and at a slower rate from 4 to 12 passes. Anomalously large grains were visible in the central region of the billet pressed through 12 passes due to dynamic recovery and grain growth. The results suggest optimum processing is achieved by pressing through 4–8 passes.     

Equal channel angular pressing of a TWIP steel: microstructure and mechanical response

A Fe–20.1Mn–1.23Si–1.72Al–0.5C TWIP steel with ultrafine grain structure was successfully processed through equal channel angular pressing (ECAP) at warm temperature up to four passes following the B _C route. The microstructure evolution was characterized by electron backscattered diffraction to obtain the grain maps, which revealed an obvious reduction in grain size, as well as a decrease in the twin fraction, with increasing number of ECAP passes. The texture evolution during ECAP was analyzed by orientation distribution function. The results show that the annealed material presents brass (B) as dominant component. After ECAP, the one pass sample presents A ₁* and A ₂* as the strongest components, while the two passes and four passes samples change gradually toward \( B/\bar{B} \) components. TEM analysis shows that all samples present twins. The twin thickness is reduced with increasing the number of ECAP passes. Nano-twins, as a result of secondary twinning, are also observed in the one and two passes samples. In the four passes sample, the microstructure is extensively refined by the joint action of ultrafine subgrains, grains and twins. The mechanical behavior was studied by tensile samples, and it was found that the yield strength and the ultimate tensile strength are significantly enhanced at increasing number of ECAP passes. Although the ductility and strain hardening capability are reduced with ECAP process, the present TWIP steel shows significant uniform deformation periods with positive work hardening rates.     

Effect of equal channel angular pressing on grain refinement and texture evolution in a biomedical alloy Ti13Nb13Zr

Evolution of texture and concomitant grain refinement during Equal Channel Angular Pressing (ECAP) of Ti13Nb13Zr alloy has been presented. Sub-micron sized equiaxed grains with narrow grain size distribution could be achieved after eight pass at 873 K. A characteristic ECAP texture evolved in α phase till four passes while the evolution of characteristic ECAP texture in the β phase could be observed only beyond the fourth pass. On increasing the deformation up to eight passes, the texture in α phase weakens while the β phase shows an ideal ECAP texture. A weaker texture, low dislocation density and high crystallite size values in α phase suggest the occurrence of dynamic recrystallization. The absence of texture evolution in β phase till four passes can be attributed to local lattice rotations. The characteristic ECAP texture in the eight pass deformed sample is attributed to delayed dynamic recrystallization in the β phase.     

Grain refinement in as cast Al–Mg–Mn alloy during high temperature equal channel angular pressing

Abstract

An as cast Al–Mg–Mn alloy with coarse equiaxed grain structure was processed by equal channel angular pressing (ECAP) at 350°C up to eight passes. Systematic studies were made on the microstructural evolution during ECAP by optical microscopy, electron backscattered diffraction and TEM. Equal channel angular pressing led to a considerable grain refinement, resulting in an average cell size of about 1 μm and a fraction of high angle boundaries of 75% after eight pressing passes. Deformation bands were not developed during the ECAP process, and a reasonably equiaxed substructure was obtained even after one pass. The main mechanism of grain refinement was attributed to the continuous dynamic recrystallisation based on the motion of deformation induced dislocations. Discontinuous recrystallisation at grain boundaries and triple junctions also contributed to the refinement, which played an important role especially at high strain of eight passes.