The processing of ultrafine-grained materials through the application of severe plastic deformation

The application of severe plastic deformation (SPD) to bulk metals provides the opportunity of achieving grain sizes in the submicrometer and nanometer range. Several different SPD processing techniques are now available including Equal-Channel Angular Pressing (ECAP), High-Pressure Torsion (HPT) and Accumulative Roll-Bonding (ARB). This paper examines the principles of grain refinement using ECAP and gives examples of the advantageous properties that may be achieved including increased strength at ambient temperatures and a superplastic forming capability at elevated temperatures. Invited paper presented in Symposium C at 5th Brazilian MRS Meeting, Florianópolis, Brazil.     

Mechanical properties and microstructure evolution in ultrafine-grained AZ31 alloy processed by severe plastic deformation

Commercial MgAlZn alloy AZ31 was processed by two techniques of severe plastic deformation (SPD)—extrusion followed by equal channel angular pressing (EX-ECAP), and high pressure torsion (HPT). Processing by ECAP was conducted at elevated temperature of 180 °C for 1–12 passes following route B_C. HPT was applied at room temperature, and the specimens of the diameter of 19 mm with different number of turns (N = ¼ ? 15) were prepared. Mechanical properties and grain fragmentation with strain due to EX-ECAP and HPT were investigated by Vickers microhardness measurements and transmission electron microscopy, respectively. Variations in dislocation density were investigated by positron annihilation spectroscopy. Differences in microhardness, grain refinement and dislocation density evolution resulting from principal differences of straining were found in the specimens. EX-ECAP resulted in homogeneous microstructure throughout the specimen's cross section as early as after four passes. On the other hand, laterally inhomogeneous microstructure with gradual reduction of grain sizes from the centre towards the periphery of the disk was observed in specimens after HPT. This microstructure and microhardness inhomogeneities were continuously smeared out and almost homogeneous ultrafine-grained structure was observed in specimen subjected to 15 HPT turns. Variations in mechanical properties and dislocation density evolution were compared in conditions corresponding to the same equivalent strain imposed by both techniques of SPD.     

大塑性变形制备超细晶/纳米晶Al-Mg铝合金的研究进展

近年来,大塑性变形(SPD)制备具有先进结构和功能的超细晶和纳米晶Al-Mg铝合金的研究取得了很大进展。SPD后,合金的晶粒显著细化、位错密度提高及有非平衡晶界和晶界偏析形成,这些微观结构导致合金的强度、硬度大幅提高。然而,SPD合金的塑性普遍较低。综述了SPD制备的Al-Mg铝合金在结构和性能方面的一些最新研究成果。     

Enhancement of mechanical properties of biocompatible Ti–45Nb alloy by hydrostatic extrusion

β-Type titanium alloys are promising materials for orthopaedic implants due to their relatively low Young’s modulus and excellent biocompatibility. However, their strength is lower than those of α- or α + β-type titanium alloys. Grain refinement by severe plastic deformation (SPD) techniques provides a unique opportunity to enhance mechanical properties to prolong the lifetime of orthopaedic implants without changing their chemical composition. In this study, β-type Ti–45Nb (wt%) biomedical alloy in the form of 30 mm rod was subjected to hydrostatic extrusion (HE) to refine the microstructure and improve its mechanical properties. HE processing was carried out at room temperature without intermediate annealing in a multi-step process, up to an accumulative true strain of 3.5. Significant microstructure refinement from a coarse-grained region to an ultrafine-grained one was observed by optical and transmission electron microscopy. Vickers hardness measurements (HV_0.2) demonstrated that the strength of the alloy increased from about 150 to 210 HV_0.2. Nevertheless, the measurements of Young’s modulus by nanoindentation showed no significant changes. This finding is substantiated by X-ray diffraction analyses which did not exhibit any phase transformation out of the bcc phase being present still before processing by HE. These results thus indicate that HE is a promising SPD method to obtain significant grain refinement and enhance strength of β-type Ti–45Nb alloy without changing its low Young’s modulus, being one prerequisite for biomedical application.     

Mechanical properties and microstructure evolution in an aluminum 6082 alloy processed by high-pressure torsion

A commercial aluminum 6082 alloy was used to investigate the effect of the initial condition on subsequent processing by high-pressure torsion (HPT). The alloy was prepared in two different initial conditions: (i) in a T651 annealed condition and (ii) after a solution treatment followed by over-aging and subsequent processing by equal-channel angular pressing (ECAP). All samples were processed by HPT through 1/2, 1, 2, 5, and 10 turns and then the microstructures were examined using electron backscattered diffraction (EBSD). Significant grain refinement was achieved after processing by HPT through 5 turns with measured grain sizes of ~0.5 μm in both types of alloy. Microhardness measurements were conducted to evaluate the evolution of hardness after HPT for the two initial conditions. It is demonstrated that there is a difference in the hardness values between these two initial conditions, and this difference remains almost constant after processing by HPT.     

Recycling of titanium machining chips by severe plastic deformation consolidation

It has been demonstrated that severe plastic deformation (SPD) can be used to consolidate particles of a wide range of sizes from nano to micro into fully dense bulk material with good mechanical properties. SPD consolidation allows processing to be conducted at much lower temperatures and is therefore suitable for particles with highly metastable structures such as nanocrystalline. It is especially useful in the fabrication of multiphase materials including metal matrix nanocomposites. In this investigation, SPD consolidation was applied to recycle Ti machining chips. In particular, the as-received chips were consolidated by equal channel angular pressing at temperatures between 400 and 600 °C with the application of a back pressure from 50 to 200 MPa. Fully dense bulk Ti with fine grain sizes was produced, possessing strength comparable or higher than that of commercially pure wrought Ti. It is concluded that SPD consolidation is a promising method for recycling and value-adding of Ti chips.     

The ductile to brittle transition of ultrafine-grained Armco iron: an experimental study

Fracture toughness measurements on bcc iron (Armco-iron), which is subjected to severe plastic deformation (SPD), were performed. Through high pressure torsion, an ultrafine grain structure was obtained and with subsequent heat treatments the grain size varied between 300 nm and 5 μm. The combination of SPD and individual heat treatments allows for a systematic study of the ductile to brittle transition (DBT) in the fracture behaviour as a function of grain size. Additionally, the influence of different crack plane orientations was taken into account. The results show that the DBT moves for smaller grain sizes (<1 μm) to higher transition temperatures. Furthermore, large differences in the absolute toughness values for a given temperature for the different crack plane orientations and grain sizes were determined. The findings can be related to a change in the crack path from transcrystalline fracture for grain sizes larger than 1 μm to intercrystalline-dominated fracture for grain sizes smaller than 1 μm.     

Different models of hardness evolution in ultrafine-grained materials processed by high-pressure torsion

High-pressure torsion (HPT) is an attractive processing method in severe plastic deformation techniques involving the application of high compressive pressure with concurrent torsional straining. Excellent grain refinement is anticipated when using this technique to average grain sizes of the submicrometer or even nanometer ranges. Because of the significant microstructural changes during processing, there are numerous reports showing evolution in local hardness toward homogeneity throughout a disk diameter with increasing numbers of revolutions. The achieved hardness after HPT is mostly much higher than that in the as-received condition because of exceptional grain refinement although there are a limited number of metals and alloys showing softening or weakening after HPT processing. This paper was initiated to review recent discoveries in the experimental results on hardness evolution toward homogeneity during HPT processing and discuss the different models of hardness developments with respect to imposed equivalent strain by HPT processing for a range of metals and alloys. Moreover, recent results of hardness homogeneity and heterogeneity through thicknesses of the processed disks are discussed toward a complete understanding of hardness evolution in the UFG metals processed by HPT.     

A comparison of microstructures and mechanical properties in a Cu–Zr alloy processed using different SPD techniques

Experiments were conducted to evaluate the microstructures and mechanical properties of a Cu–0.1 % Zr alloy processed using two different techniques of severe plastic deformation: equal-channel angular pressing (ECAP) and high-pressure torsion (HPT). The samples were processed at room temperature through ECAP for eight passes or through HPT for 10 turns. The results show HPT is more effective both in refining the grains and in producing a large fraction of grain boundaries having high angles of misorientation. Both procedures produce reasonably homogeneous hardness distributions but the average hardness values were higher after HPT. In tensile testing at 673 K, the highest strength and ductility was achieved after processing by HPT. This is attributed to the grain stability and high fraction of high-angle grain boundaries produced in HPT.     

Tribological properties of ultrafine-grained materials processed by severe plastic deformation

Processing by severe plastic deformation (SPD) has been developed extensively over the last two decades in order to produce ultrafine-grained (UFG) materials having submicrometre or nanometre grain sizes. An important material property for UFG materials is good wear resistance so that they may be used in a range of structural applications. An examination of the published data shows that only limited reports are available to date on the wear behaviour of SPD-processed materials and, furthermore, many of these results appear to be conflicting. The correlation of hardness and wear is limited because the wear property is a system property that in practice is influenced by a range of factors. Accordingly, this review is designed to examine recent reports related to the wear resistance of materials processed by SPD with particular emphasis on alloys processed using equal-channel angular pressing (ECAP), high-pressure torsion (HPT) and accumulative roll-bonding (ARB).     

Evolution of microhardness and microstructure in a cast Al–7 % Si alloy during high-pressure torsion

Disks of a cast Al–7 % Si alloy were processed through high-pressure torsion (HPT) for 1/4, 1/2, 1, 5, and 10 revolutions under a pressure of 6.0 GPa and at temperatures of 298 and 445 K. The hardness of the samples after processing was significantly higher than in the cast sample, and the hardness profiles across the samples became more uniform with increasing numbers of turns. Processing at higher temperature gave lower hardness values. Experiments were conducted to examine the effects of HPT processing on various microstructural aspects of the cast Al–7 % Si alloy such as the grain size, the Taylor factor, and the fraction of high-angle grain boundaries. The results demonstrate that there is a correlation between trends in the microhardness values and the observed microstructures.     

Solid state crack repair by friction stir processing in 304L stainless steel

Friction stir processing (FSP) was investigated as a method of repairing cracks in 12 mm thick 304L stainless steel plate. Healing feasibility was demonstrated by processing a tapered crack using a PCBN/W-Re tool with a 25 mm diameter shoulder and a pin length of 6.4 mm. The experiment showed that it was possible to heal a crack that begins narrow and then progressively grows up to a width of 2 mm. Bead on plate experiments were used to find the best parameters for creating a consolidated stir zone with the least amount of hardness difference compared to the base metal. Grain refinement in some specimens resulted in much higher stir zone hardness, compared to base metal. A plot of grain size versus microhardness showed a very strong inverse correlation between grain size and hardness, as expected from the Hall-Petch relationship. Corrosion testing was carried out in order to evaluate the effect of FSP on potential sensitization of the stir zone. After 1000 h of intermittent immersion in 3.5% saline solution at room temperature it was found that no corrosion products formed on the base material controls or on any of the friction stir processed specimens.     

Recent development in grain refinement by hydrostatic extrusion

Hydrostatic extrusion is an efficient method of grain refinement to the nanometer scale in metallic materials. The paper shows that it can be used directly to obtain a mean grain size smaller than 100 nm with a significant fraction of high angle grain boundaries in aluminum alloys, titanium, and iron. It is also demonstrated that grain size reduction to this level in some other materials, e.g., nickel, requires a combination of hydrostatic extrusion (HE), as the final operation, after some other methods of severe plastic deformation (SPD). Grain refinement in metallic materials by HE has a significant effect on their properties with a significant increase in mechanical strength and improvement of wear and corrosion resistance while maintaining an acceptable level of plasticity.     

Machine Learning Based Predictive Modeling of Machining Induced Microhardness and Grain Size in Ti–6Al–4V Alloy

Titanium and its alloys are today used in many industries including aerospace, automotive, and medical device and among those Ti–6Al–4 V alloy is the most suitable because of favorable properties such as high strength-to-weight ratio, toughness, superb corrosion resistance, and bio-compatibility. Machining induced surface integrity and microstructure alterations size play a critical role in product fatigue life and reliability. Cutting tool geometry, coating type, and cutting conditions can affect surface and subsurface hardness as well as grain size. In this paper, predictions of machining induced microhardness and grain size are performed by using 3D finite element (FE) simulations of machining and machine learning models. Microhardness and microstructure of machined surfaces of Ti–6Al–4 V are investigated. Hardness measurements are conducted at elevated temperatures to develop a predictive model by utilizing FE-based temperature fields for hardness profile. Measured hardness, grain size, and fractions are utilized in developing predictive models. Predicted microhardness profiles and grain sizes are then utilized in understanding the effect of machining parameters such as cutting speed, tool coating, and edge radius on the surface integrity. Optimization using genetic algorithms is performed to identify most favorable tool edge radius and cutting conditions.     

Microstructural evolution in ultrafine-grained titanium processed by high-pressure torsion under different pressures

A grade 2 commercially pure (CP) titanium was processed by high-pressure torsion (HPT) at pressures of 3.0 and 6.0 GPa in order to achieve improved strengths. The microhardness values for these Ti samples were plotted against the imposed strain, and the plots show that a higher saturation microhardness of 320 Hv is achieved for the sample processed at 6.0 GPa compared to a microhardness of 305 Hv when using a pressure of 3.0 GPa. The omega ω-phase has been reported in some earlier HPT investigations of pure titanium, but it was not detected in this investigation even after processing at 6.0 GPa. The absence of the ω-phase is attributed to the relatively high level of oxygen (0.25 wt%) in these CP titanium samples. The higher saturation hardness for the 6.0 GPa sample is consistent with the smaller average grain size of ~105 ± 12 nm compared with the measured grain size of ~130 ± 18 nm after processing with an imposed pressure of 3.0 GPa.     

Comparison study of silicon carbide coatings produced at different deposition conditions with use of high temperature nanoindentation

The elastic modulus and hardness of different silicon carbide (SiC) coatings in tristructural-isotropic (TRISO) fuel particles were measured by in situ high temperature nanoindentation up to 500 °C. Three samples fabricated by different research institutions were compared. Due to varied fabrication parameters the samples exhibited different grain sizes and one contained some visible porosity. However, irrespective of the microstructural features in each case the hardness was found to be very similar in the three coatings around 35 GPa at room temperature. Compared with the significantly coarser grained bulk CVD SiC, the drop in hardness with temperature was less pronounced for TRISO particles, suggesting that the presence of grain boundaries impeded plastic deformation. The elastic modulus differed for the three TRISO coatings with room temperature values ranging from 340 to 400 GPa. With increasing measurement temperature the elastic modulus showed a continuous decrease.     

Evolution of strength and structure during SPD processing of Ti–45Nb alloys: experiments and simulations

A β-phase Ti–45Nb alloy was processed by several severe plastic deformation (SPD) methods as high-pressure torsion, cold rolling and folding, and hydrostatic extrusion to enhance its strength by achieving an ultrafine grained structure without affecting the Young’s modulus being close to that of bone material. Mechanical properties during processing were monitored by direct torque and Vickers hardness measurements, while the micro-/nano-structural evolution was investigated by transmission electron microscopy and X-ray line profile analysis. Simulations of both mechanical and micro-/nano-structural data were performed on the basis of the SPD work-hardening model by Zehetbauer. The simulations not only found a good agreement with the deformation-specific evolution of strength and density of individual dislocations but also well reflected mesoscopic structural quantities such as the sizes of cell/grain interiors and walls without introducing additional fitting parameters.     

Interpretation of hardness evolution in metals processed by high-pressure torsion

The processing of metals through the application of high-pressure torsion (HPT) provides the potential for achieving exceptional grain refinement in bulk disks. Numerous reports are now available describing the application of HPT to a range of pure metals and simple alloys. Excellent grain refinement was achieved using this processing technique with the average grain size often reduced to the nanoscale range. By contrast, the development of microstructure and local hardness is different depending upon the material properties. In order to make HPT processing more practical, it is indispensable to investigate the nature of the sample characteristics immediately after conventional HPT processing. Accordingly, this report demonstrates the different models of hardness evolution using representative materials of AZ31 magnesium alloy, high-purity aluminum, and Zn–22 % Al eutectoid alloy processed by HPT. Separate models are described for the evolution of hardness with equivalent strain, and the correlation between these models is suggested by the homologous temperature of HPT processing. A special emphasis is placed on examining the numerical expression of the level of strain hardening or softening of these metals with increasing equivalent strain.     

Investigation of friction stir processing effect on AA 2014-T6

This study is concerned with the effects of process parameters such as speed, feed, tilt angle, and tool profile on mechanical and microstructural properties of stir processed, solution treated, and artificially aged AA 2014-T6. The process was carried out with an input condition at rotational and traverse feeds of 600–1400 RPM and 30–90 mm/min, respectively. Five distinct shapes of the tool pin such as triangular, hexagonal, threaded, conical, and cylindrical have been selected to carry out the process with varied tilt angle of 1°–3°. In order to exemplify the status of processed materials, optical, scanning electron microscopy and Vickers hardness measurement along with grain analysis were performed on various regions of processed cross sections. According to the results, combination of processing speed and rotational speed affects the microstructure and associated grain size and average hardness of the processed region.     

The new trends in fabrication of bulk nanostructured materials by SPD processing

During the past decade, fabrication of bulk nanostructured metals and alloys using severe plastic deformation (SPD) has been evolving as a rapidly advancing direction of nanomaterials science and technology aimed at developing materials with new mechanical and functional properties for advanced applications. The principle of these developments is based on grain refinement down to the nanoscale level via various SPD techniques. This paper is focused on investigation and development of new SPD processing routes enabling fabrication of fully dense bulk nanostructured metals and alloys with a grain size of 40–50 nm and smaller, namely, SPD-consolidation of powders, including nanostructured ones, as well as SPD-induced nanocrystallization of amorphous alloys. We also consider microstructural features of SPD-processed materials that are responsible for enhancement of their properties.