The Role of Carbon in Grain Refinement of Cast CrFeCoNi High-Entropy Alloys

As a promising engineering material, high-entropy alloys (HEAs) CrFeCoNi system has attracted extensive attention worldwide. Their cast alloys are of great importance because of their great formability of complex components, which can be further improved through the transition of the columnar to equiaxed grains and grain refinement. In the current work, the influence of C contents on the grain structures and mechanical properties of the as-cast high-entropy alloy CrFeCoNi was chosen as the target and systematically studied via a hybrid approach of the experiments and thermodynamic calculations. The alloys with various C additions were prepared by arc melting and drop cast. The as-cast macrostructure and microstructure were characterized using optical microscopy, scanning electron microscopy, and transmission electron microscopy. The cast HEAs transform from coarse columnar grains into equiaxed grains with the C level increased to ≥ 2 at. pct and the size of equiaxed grains is further decreased with the increasing C addition. It is revealed that the interdendritic segregation of Cr and C results in grain boundary precipitation of M₂₃C₆ carbides. The grain refinement is attributed to the additional constitutional supercoiling from the C addition. The yield stress and tensile strength at room temperature are improved due to the transition of columnar to equiaxed grains and grain refinement.     

Deformation Mechanisms in the Near-β Titanium Alloy Ti-55531

The hot formability of a near-β titanium alloy is studied near the β transus temperature to determine the mechanisms of deformation. Compression tests of Ti-5Al-5Mo-5V-3Cr-1Zr are carried out using a Gleeble^®1500 device between 1036 K and 1116 K (763 °C and 843 °C) and strain rates between 0.001 and 10 s^?1. The achieved flow data are used to calculate the efficiency of power dissipation, the strain rate sensitivity, and instability parameters derived from different models. Constitutive equations are built using the stress values at the strain of 0.4. Light optical microscopy and EBSD measurements are used to correlate the parameters that describe formability with the microstructure. It is found that hot deformation is achieved by dynamic recovery in the β phase by subgrain formation. Geometric dynamic recrystallization along the β grain boundaries takes place at large deformations, high temperatures, and low strain rates. On the other hand, for high strain rates, continuous dynamic recrystallization by lattice rotation already starts at a local strain of 1. Different phenomenological models are used to predict the flow instabilities, where the flow-softening parameter α _i provides the best correlation with microstructure as well as the physical understanding. The instabilities observed in this alloy are strongly related to flow localization by adiabatic heat.     

Formability behavior of brass alloy sheet: the role of twins in microstructure

Quantitative understanding of the process and formability parameters involved in grain size and the formation of annealing twins after plastic straining is important in the control of the manufacturing process. There is a synergistic effect of strain and temperature on the density of annealing twins. Formability of brass alloy sheets was studied after annealing of 65% cold worked (CW) samples at different temperatures (300–600°C). Tensile, deep drawing and Erichsen tests were carried out at room temperature to evaluate formability of alloy. Effect of annealing temperature on density, distribution and size of twins is investigated. It was shown that annealing of brass alloy resulting in formation of annealing twins which at higher annealing temperature were reduced by increasing grain size. Best deep drawability would be achieved by annealing at moderate temperature 400–450°C which microstructure consists of fine grain and twin bands. Work hardening exponent of samples was calculated based on the tensile test data and correlated with stretch ability of annealed brass sheets. It was found that the sheets annealed at 600°C possess best ductility and high average n-value.     

Microstructure and Mechanical Properties of Ultrafine-Grained Interstitial-Free Steel Processed by ECAP

Equal-channel angular pressing (ECAP) of interstitial-free (IF) steel at equivalent strain, ε_vm = 12 has been employed to develop ultrafine-grained (UFG) microstructure with high fraction of low angle grain boundaries, that enhances strength significantly with reduced tensile ductility. ECAPed IF steel has been deformed further by cold rolling/cryorolling at ?50 °C to >90 % reduction in area. It is observed that the UFG structure gets refined with an improvement in high angle grain boundary fraction and heavily stressed non-equilibrium grain boundaries in cryorolled state resulting in significant strengthening. However, the decrease in grain size to an ultrafine level with the increased lattice strain lowers the work hardening ability of the material that limits its ductility. Hence, the rolled samples are flash annealed at 675 °C in order to recover the ductility of the material by achieving partially recrystallized structures. Consequently, the increased subgrain size as well as the grain size, the reduced residual lattice strain, lower hardness and strength with marginal recovery of ductility is maintained in order to attain the yield strength 2–3 times compared to that of as-received coarse-grained IF steel.     

The effect of grain size, strain rate, and temperature on the mechanical behavior of commercial purity aluminum

Commercial purity aluminum AA1050 was subjected to equal channel angular extrusion (ECAE) that resulted in an ultrafine-grained (UFG) microstructure with an as-received grain size of 0.35 μm. This UFG material was then annealed to obtain microstructures with grain sizes ranging from 0.47 to 20 μm. Specimens were compressed at quasi-static, intermediate, and dynamic strain rates at temperatures of 77 and 298 K. The mechanical properties were found to vary significantly with grain size, strain rate, and temperature. Yield stress was found to increase with decreasing grain size, decreasing temperature, and increasing strain rate. The work hardening rate was seen to increase with increasing grain size, decreasing temperature, and increasing strain rate. The influence of strain rate and temperature is most significant in the smallest grain size specimens. The rate of work hardening is also influenced by strain rate, temperature, and grain size with negative rates of work hardening observed at 298 K and quasi-static strain rates in the smallest grain sizes and increasing rates of work hardening with increasing loading rate and grain size. Work hardening behavior is correlated with the substructural evolution of these specimens.     

Bulk Nanolaminated Nickel: Preparation,Microstructure, Mechanical Property,and Thermal Stability

A bulk nanolaminated (NL) structure with distinctive fractions of low- and high-angle grain boundaries (f _LAGBs and f _HAGBs) is produced in pure nickel, through a two-step process of primary grain refinement by equal-channel angular pressing (ECAP), followed by a secondary geometrical refinement via liquid nitrogen rolling (LNR). The lamellar boundary spacings of 2N and 4N nickel are refined to ~ 40 and ~ 70 nm, respectively, and the yield strength of the NL structure in 2N nickel reaches ~ 1.5 GPa. The impacts of the deformation path, material purity, grain boundary (GB) misorientation, and energy on the microstructure, refinement ability, mechanical strength, and thermal stability are investigated to understand the inherent governing mechanisms. GB migration is the main restoration mechanism limiting the refinement of an NL structure in 4N nickel, while in 2N nickel, shear banding occurs and mediates one-fifth of the total true normal rolling strain at the mesoscale, restricting further refinement. Three typical structures [ultrafine grained (UFG), NL with low f _LAGBs, and NL with high f _LAGBs] obtained through three different combinations of ECAP and LNR were studied by isochronal annealing for 1 hour at temperatures ranging from 433 K to 973 K (160 °C to 700 °C). Higher thermal stability in the NL structure with high f _LAGBs is shown by a 50 K (50 °C) delay in the initiation temperature of recrystallization. Based on calculations and analyses of the stored energies of deformed structures from strain distribution, as characterized by kernel average misorientation (KAM), and from GB misorientations, higher thermal stability is attributed to high f _LAGBs in this type of NL structure. This is confirmed by a slower change in the microstructure, as revealed by characterizing its annealing kinetics using KAM maps.     

Microstructure and Strengthening Mechanisms in an Ultrafine Grained Al-Mg-Sc Alloy Produced by Powder Metallurgy

Additions of Sc to an Al-Mg matrix were investigated, paying particular attention to the influence of Al₃Sc precipitates and other dispersoids, as well as grain size, on mechanical behavior. Prior studies have shown that Sc significantly increases the strength of coarse-grained Al-Mg alloys. Prompted by these findings, we hypothesized that it would be of fundamental and technological interest to study the behavior of Sc additions to an ultrafine-grained (UFG) microstructure (e.g., 100’s nm). Accordingly, we investigated the microstructural evolution and mechanical behavior of a cryomilled ultrafine grained Al-5Mg-0.4Sc (wt pct) and compared the results to those of an equivalent fine-grained material (FG) produced by powder metallurgy. Experimental materials were consolidated by hot isostatic pressing (HIP’ing) followed by extrusion or dual mode dynamic forging. Under identical processing conditions, UFG materials generate large Al₃Sc precipitates with an average diameter of 154 nm and spaced approximately 1 to 3 μm apart, while precipitates in the FG materials have a diameter of 24 nm and are spaced 50 to 200 nm apart. The strengthening mechanisms are calculated for all materials and it is determined that the greatest strengthening contributions for the UFG and FG materials are Mg-O/N dispersion strengthening and precipitate strengthening, respectively.     

Enhanced Mechanical Properties of As-Forged Co-Cr-Mo-N Alloys with Ultrafine-Grained Structures

The ultrafine-grained (UFG) microstructures of Ni-free Co-29Cr-6Mo (mass pct) alloys, which are designed for biomedical applications, have been successively fabricated by the conventional hot-forging process. The grain size decreased with increasing hot-forging reduction, and the equiaxed UFG structures with a mean grain size less than 1 ??m were obtained in 83?pct (true strain of 1.8) hot-forged specimens. Significant grain refinement drastically enhanced tensile strength; dislocations residual in the grains also play a crucial role for strengthening of the UFG-structured specimen. The elongation decreased with the reduction in grain size. However, we revealed that the addition of nitrogen, which is one of the nontoxic ?? phase (face-centered cubic [fcc] structure) stabilizer, improves the ductility of the UFG alloys remarkably with maintaining high strength. It was deduced that the enhanced ductility in the UFG material by N doping was related to constituent phase and strain-induced martensitic transformation behavior: the addition of nitrogen eliminated athermal ?? martensite detrimental to tensile elongation, and strain-induced martensitic transformation effectively increased work-hardening rate to avoid the plastic instability at the early stage of deformation. The present method characterized by ultragrain refinement in conjunction with nitrogen addition to stabilize the ?? phase can provide a potent strategy to obtain superior combination of high strength and adequate ductility.     

Microstructural Evolution and Mechanical Response of Equal-Channel Angular Extrusion-Processed Al-40Zn-2Cu Alloy

Microstructural evolution, tensile properties, and impact toughness of an aluminum-zinc-copper (Al-40Zn-2Cu) alloy subjected to repetitive equal-channel angular extrusion (ECAE) up to four passes following either route A or route B_C were investigated. The experimental results reveal that the ECAE eliminated as-cast dendritic microstructure along with casting defects such as microporosities almost completely. The ECAE-processed samples consisted of mostly elongated microconstituents via route A and equiaxed microconstituents via route B_C. The high stresses imposed in ECAE lead to the fragmentation of the copper-rich θ phase into smaller particles with significant fragmentation occurring in the first pass and additional breaking in the subsequent passes in both routes. The ECAE processing simultaneously increased both the strength and ductility of the alloy as compared to the as-cast state, regardless of the processing route and number of passes. The deformation behavior of as-cast Al-40Zn-2Cu alloy has changed from brittle to ductile mode after ECAE due to the microstructural refinement, deformation-induced homogenization, and reduction of porosities. The limited impact toughness of as-cast alloy was significantly improved by multipass ECAE, especially in route A.     

TEM studies on recovery and recrystallisation in Equal Channel Angular Extrusion processed Al-3%Mg alloy

Equal Channel Angular Extrusion (ECAE) is a promising severe plastic deformation (SPD) process which can produce polycrystalline materials with ultra-fine grains (UFG) of sub micrometer range or nanometer range. Large plastic shear deformation induced by the high applied pressure in ECAE material processing is the prime reason behind the grain refinement. The focus of the present work is to study the evolution of dislocation microstructure during dynamic recovery (due to intense strain deformation) and static recovery (due to static annealing after deformation) in commercial Al-3%Mg alloy processed by ECAE. It is observed that local concentrations of shear strain can take place and high angle boundary (HAGB) segments are formed initially at random locations. When thermal energy is provided, during static annealing, the boundary segments get further defined and extended. This leads to the formation of very fine size grains with high mis-orientations which subsequently develop into an ultra-fine grain distribution in the material. Also, it appears dynamic recrystallisation (DRX) occurring during the deformation itself is a general phenomenon leading to refinement of grains. Transmission Electron Microscopy (TEM) is the characterizing tool used in the present study. The influence of precipitates/second phase particles on the deformation characteristics and on the increased degree of grain fragmentation is also detailed.     

Warm Formability of 0.2 Pct C-1.5 Pct Si-5 Pct Mn Transformation-Induced Plasticity-Aided Steel

The warm stretch formability and flangeability of 0.2 pct C-1.5 pct Si-5 pct Mn transformation-induced plasticity-aided sheet steel with annealed martensite matrix were investigated for automotive applications. Both formabilities were enhanced by warm forming at peak temperatures of 423 K to 573 K and 423 K to 523 K (150 °C to 300 °C and 150 °C to 250 °C), respectively. The superior warm formabilities were mainly due to the stabilization of a large amount of retained austenite by warm forming and the consequent considerably suppressed void growth at the interface between the matrix and transformed martensite, despite there being large hole punching damage for the stretch flangeability. High peak temperatures for stretch formability and flangeability were associated with apparently increased M _S of the retained austenite resulting from the increased mean normal stress on stretch forming and hole expansion.     

Microstructure and Mechanical Properties of Oxide-Dispersion Strengthened Al6063 Alloy with Ultra-Fine Grain Structure

The microstructure and mechanical properties of the ultra-fine grained (UFG) Al6063 alloy reinforced with nanometric aluminum oxide nanoparticles (25 nm) were investigated and compared with the coarse-grained (CG) Al6063 alloy (~2 μm). The UFG materials were prepared by mechanical alloying (MA) under high-purity Ar and Ar-5 vol pct O₂ atmospheres followed by hot powder extrusion (HPE). The CG alloy was produced by HPE of the gas-atomized Al6063 powder without applying MA. Electron backscatter diffraction under scanning electron microscopy together with transmission electron microscopy studies revealed that the microstructure of the milled powders after HPE consisted of ultra-fine grains (>100 nm) surrounded by nanostructured grains (<100 nm), revealing the formation of a bimodal grain structure. The grain size distribution was in the range of 20 to 850 nm with an average of 360 and 300 nm for Ar and Ar-5 pct O₂ atmospheres, respectively. The amount of oxide particles formed by reactive mechanical alloying under the Ar/O₂ atmosphere was ~0.8 vol pct, whereas the particles were almost uniformly distributed throughout the aluminum matrix. The UFG materials exhibited significant improvement in the hardness and yield strength with an absence of strain hardening behavior compared with CG material. The fracture surfaces showed a ductile fracture mode for both CG and UFG Al6063, in which the dimple size was related to the grain structure. A mixture of ductile–brittle fracture mode was observed for the UFG alloy containing 0.8 vol pct Al₂O₃ particles. The tensile behavior was described based on the formation of nonequilibrium grain boundaries with high internal stress and dislocation-based models.     

Grain Refinement in Pure Aluminum Severely Deformed by Equal Channel Angular Extrusion via Extended Processing Routes

AA1060 pure aluminum billets were processed by eight passes of equal channel angular extrusion (ECAE) using 90 and 120 deg dies via processing routes characterized by an inter-pass billet rotation angle (χ) varying from 0 to 180 deg. The grain refinement efficiencies achieved in the different processing conditions were investigated by comparing misorientation and grain size in the deformed samples measured by electron back-scatter diffraction. The results reveal an overall decrease of grain refinement efficiency with an increase of χ for both dies. This trend corroborates the general observations in various face-centered cubic metals processed using a 120 deg die and can be satisfactorily explained by correlating the relative grain refinement efficiency to the relative significance of newly activated slip systems at pass-to-pass transitions. For ECAE with the 90 deg die, the route-dependency of grain refinement found in the AA1060 samples contradicts some of the observations in the literature, and the main discrepancies are located for routes with χ = 0 to 90 deg. Comparison of the present results with those of pure copper processed under similar conditions further reveals that these discrepancies could be mainly ascribed to differences in the characteristics of the materials, and that it is irrational to simply claim the route with χ = 0 or 90 deg as the optimal route without necessary experimental validations for a specific material.     

Biaxial Deformation Behavior and Enhanced Formability of Ultrafine-Grained Pure Copper

Coarse-grained commercially pure Cu was subjected to equal channel angular pressing at room temperature for 2 passes and 12 passes resulting in grain refinement down to the ultrafine scale. Uniaxial tensile testing revealed that as-ECAP Cu samples have very high strength, but low uniform elongation and elongation to failure, whereas small punch testing showed that strain in biaxial stretching of the as-ECAP Cu specimens was comparable to that in the coarse-grained Cu. Analysis of surface relief demonstrated extensive microlocalization of plastic flow into microshear bands during biaxial stretching of the as-ECAP Cu specimens. The effect of microstructure and stress state on formability of the material and the mechanisms governing its plastic deformation are discussed. It is suggested that although the high strength as-ECAP Cu exhibits poor ductility in uniaxial tension, in other strain paths such as biaxial stretching, it can show high formability which is sufficient for metal-forming processes.     

Hot working of Ti-6Al-4V via equal channel angular extrusion

The deformation behavior of Ti-6Al-4V during high-temperature equal channel angular extrusion (ECAE) with or without an initial increment of upset deformation was determined for billets with either a lamellar or an equiaxed alpha preform microstructure. For conventional ECAE (i.e., deformation by simple shear alone), flow localization and fracture occurred at temperatures between 900 °C and 985 °C. In contrast, billets deformed at temperatures between 845 °C and 985 °C using an initial increment of upset deformation immediately followed by the simple shear deformation of ECAE exhibited uniform flow with no significant cracking or fracture. A simple flow-localization criterion was used to explain the influence of preupsetting on the suppression of localization in billets with the lamellar microstructure. The suppression of flow localization for the equiaxed microstructure and the elimination of edge cracking for both types of microstructures were explained in terms of heat transfer (die chill) and workpiece geometry. Further evidence of the relative importance of microstructural and thermal effects was extracted from the results of two-pass extrusions, the first with upsetting and the second without upsetting.     

Effect of the severe plastic deformation temperature on the diffusion properties of the grain boundaries in ultrafine-grained metals

A model is proposed to explain the effect of the severe plastic deformation (SPD) temperature on the diffusion properties of the grain boundaries in ultrafine-grained (UFG) metals and alloys. It is shown that an increase in the SPD temperature in UFG metals leads to an increase in the activation energy of grainboundary diffusion from (3–5)k _B T _m, which corresponds to the diffusion parameters of nonequilibrium grain boundaries, to (8–10)k _B T _m, which corresponds to the diffusion parameters of equilibrium grain boundaries (k _B is the Boltzmann constant, T _m is the melting temperature). The dependence of the activation energy of grain-boundary diffusion on the SPD temperature is found to be determined by the kinetics of the competing processes of defect accumulation at grain boundaries and the diffusion accommodation of defects.     

Ultrafine-Grained Al-Mg-Sc Alloy via Friction-Stir Processing

Friction-stir processing (FSP) of twin-roll cast (TRC) Al-Mg-Sc alloy resulted into ultrafine-grained microstructure. The alloy was processed in as-received and aged (563 K [290 °C], 22 hours) conditions and at three different tool rotation rates: 800, 400, and 325 rpm. The microstructural features were characterized using electron backscattered diffraction (EBSD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The grain size varied from 0.89 μm to 0.39 μm depending on the processing and initial thermo-mechanical conditions of the alloy. The TRC alloy processed at 325 rpm in aged condition had all the grains less than 1 μm, and 95 pct of grains had high-angle grain boundaries (HAGBs). In all the cases, the fraction of HAGBs were more than 80 pct. The variation of misorientation angle distribution was similar to the theoretical MacKenzie distribution for cubic crystal materials. Grain size analysis at different sections and locations on the transverse section of the dynamically recrystallized zone showed a homogeneous and equiaxed microstructure. The average dispersoid (Al₃(Sc,Zr)) size was ~8.0 nm in diameter obtained using high-resolution TEM. Grain size reduction was observed with increase in Zener–Hollomon parameter. It was shown that under the current microstructural and deformation conditions, dynamic recrystallization via particle-stimulated nucleation might not be possible during FSP.     

Low-temperature superplasticity of ultra-fine-grained Ti-6Al-4V processed by equal-channel angular pressing

The low-temperature superplasticity of ultra-fine-grained (UFG) Ti-6Al-4V was established as a function of temperature and strain rate. The equiaxed-alpha grain size of the starting material was reduced from 11 to 0.3 μm (without a change in volume fraction) by imposing an effective strain of ∼4 via isothermal, equal-channel angular pressing (ECAP) at 873 K. The ultrafine microstructure so produced was relatively stable during annealing at temperatures up to 873 K. Uniaxial tension and load-relaxation tests were conducted for both the starting (coarse-grained (CG)) and UFG materials at temperatures of 873 to 973 K and strain rates of 5 × 10⁻⁵ to 10⁻² s⁻¹. The tension tests revealed that the UFG structure exhibited considerably higher elongations compared to those of the CG specimens at the same temperature and strain rate. A total elongation of 474 pct was obtained for the UFG alloy at 973 K and 10⁻⁴ s⁻¹. This fact strongly indicated that low-temperature superplasticity could be achieved using an UFG structure through an enhancement of grain-boundary sliding in addition to strain hardening. The deformation mechanisms underlying the low-temperature superplasticity of UFG Ti-6Al-4V were also elucidated by the load-relaxation tests and accompanying interpretation based on inelastic deformation theory.