High Pressure Torsion Deformation Research Articles

Influence of Severe Plastic Deformation on the Magnetic Properties of Sm–Co Permanent Magnets

High pressure torsion (HPT) is presented as a new fabrication route to produce bulk Sm–Co magnets with a strongly refined microstructure down to the nanometer regime. The initial powders, based on the compositions SmCo5, Sm2Co7 and Sm2Co17, are compacted and subsequently deformed by HPT. The microstructural evolution in dependence on the applied deformation parameters is characterized by electron microscopy and the effect of HPT on the phase stability is monitored by synchrotron X‐ray diffraction. An increasing amount of applied strain leads to a stronger reduction in grain size while strain localization counteracts a homogeneous microstructural refinement. The positive effect of elevated deformation temperatures is demonstrated for Sm2Co17, which promotes homogeneous grain refinement, but causes strain‐induced phase transformations at the same time, strongly affecting the magnetic behavior. Superconducting quantum interference device magnetometry is used to characterize the magnetic properties after HPT deformation, which indicates the formation of a magnetic texture depending on the respective phase.

Magnetic characterization of HPT-deformed Fe–Si soft magnetic alloys before and after heat treatment and internal stress calculations

Fe, Fe-3wt%Si, and Fe-6.5 wt%Si alloys were subjected to high-pressure torsion (HPT) to achieve a nanostructure (<100 nm grain size). HPT processing was done at 77 and 293 K and heat treatments were performed on the deformed samples to reduce internal stresses that are known to deteriorate soft magnetic properties by impeding the movement of domain walls. X-ray line profile analysis (XLPA) was used to find out the crystallite/subgrain/domain size and the dislocation density in the deformed samples. The coercivity Hc was characterized on ring-shaped samples using a hysteresisgraph. Internal stresses in the deformed and heat-treated samples were determined using magnetic data and the dislocation density data and a comparison is made between the two approaches. HPT deformation increases the coercivity of the samples while heat treatment after deformation reduces the coercivity to a certain extent in Fe samples but has mixed results in Fe–Si alloys. In comparison with Herzer's theory, zero-frequency Hc was plotted against crystallite (or subgrain) size and it was found that coercivity follows a D1.5 relation, where D is crystallite size.

Исследование усталостных свойств и трибологические испытания стали AISI 316 после кручения под высоким давлением

The effect of high-pressure torsion process in a new die on the fatigue properties of corrosion-resistant steel AISI 316 has been studied. The deformation was carried out at cryogenic and room temperatures. The number of deformation cycles was 8. The initial blank had a ring shape with a diameter of 76 mm, a width of 3.5 mm and a thickness of 3 mm. It is revealed that the fatigue strength of both samples increases due to structure refinement and twinning in austenite during high pressure torsion deformation, partial martensitic transformation and increase of the share of more angular boundaries during cyclic deformation. The main factor of higher fatigue limit of AISI 316 steel after cryogenic deformation in comparison with room temperature is more intensive grinding of microstructure and presence of increased share of large-angle boundaries and more complete martensitic transformation.

Magnetic properties of NdFeB-based alloy under high-pressure torsion

Abstract When a multicomponent NdFeB-based magnetic alloy is deformed using high-pressure torsion (HPT), a quasi-stationary state is reached after 2.5 anvil revolutions, which corresponds to an equivalent strain of ∼40 at the sample mid-radius. In this state, torque self-oscillations are observed with a period of about 1.5 s and an amplitude of ∼10 % around the average value of 550 N m−1. Such self-oscillations are accompanied by strong acoustic emission. Before HPT, the alloy under study has an almost rectangular hysteresis loop with saturation magnetization J s = 135 emu g−1 and coercivity H c = 34.8 kOe. HPT deformation at initial stages transforms this alloy to the class of soft magnets: H c drops to 1.35 × 10−4 kOe, while J s practically does not change. An increase in strain leads to a gradual increase in H c to 9.61 kOe and a decrease in J s to ∼100 emu g−1 at the number of anvil revolutions n = 7. This is explained by HPT modification of the regular grain-boundary network of neodymium-rich paramagnetic phase layers. These layers provide magnetic isolation between grains of the Nd2Fe14B ferromagnetic phase. Periodic changes in torque and J s with increasing torsion angle are caused by transitions from the amorphous phase to the crystalline one and vice versa.

Structure and cryogenic mechanical properties of severely deformed nonequiatomic alloys of Fe–Mn–Co–Cr system

The work is devoted to a study of the structure and mechanical properties of two nonequiatomic medium-entropy nanocrystalline alloys, in which in a coarse state additional mechanisms act during plastic deformation — twinning (TWIP) in the Fe40Mn40Co10Cr10 alloy and phase transformations (TRIP) in the Fe50Mn30Co10Cr10 alloy. The nanocrystalline state in these alloys is achieved by high-pressure torsion (HPT) at 300 K and 77 K after different numbers of revolutions n = 0.25 and 5. In the nanostructural state in the TWIP Fe40Mn40Co10Cr10 and the TRIP Fe50Mn30Co10Cr10 alloys, a basically complete phase transition from the fcc lattice to hcp is observed, the content of which does not depend very strongly on the HPT temperature and deformation. For both alloys in the nanostructured state, there is a significant decrease in differences in the phase composition and microhardness Hv by comparison with the coarse-grained state. A decrease in the HPT temperature and an increase in HPT deformation for all the cases studied lead to an increase in the value of Hv. The Fe40Mn40Co10Cr10 TWIP alloy remains ductile under active compression deformation at 300 and 77 K, while there is no macroscopic plasticity in the Fe50Mn30Co10Cr10 TRIP alloy under similar conditions. For the Fe40Mn40Co10Cr10 TWIP the thermally-activated character of plastic deformation is retained during the transition from the coarse-grained to the nanostructured state.

X-ray line profile analysis study on the evolution of the microstructure in additively manufactured 316L steel during severe plastic deformation

316L stainless steel was manufactured by additive manufacturing (AM), and then, the samples were severely deformed by the high-pressure torsion (HPT) technique. The evolution of the microstructure was monitored by X-ray line profile analysis. This method gives the crystallite size and the density of lattice defects, such as dislocations and twin faults. The AM-processing of the HPT disks was performed in two different modes: the laser beam was parallel or orthogonal to the normal direction of the disks. The subsequent HPT deformation was carried out for ½, 1, 5 and 10 turns. The microstructure and hardness evolution during HPT were similar regardless of the laser beam direction. For both sample series, the minimum achievable crystallite size was about 30 nm, while the dislocation density and the twin fault probability got saturated at the values of 300–350 × 1014 m−2 and 3.5–4%, respectively. The microstructure evolution during HPT of the AM-prepared 316L steel was compared with the HPT-induced changes in an as-cast counterpart. It was found that while the AM-prepared 316L steel remained a single-phase face-centered cubic γ-structure during HPT, in the as-cast samples a body-centered cubic (bcc) martensitic α-phase became the main phase with increasing the imposed strain of HPT due to the lower Ni content. In the saturation state achieved by HPT the initially as-cast 316L steel had a considerably higher hardness (about 6000 MPa) than that for the AM-prepared samples (~ 5000 MPa) due to the large fraction of the hard bcc phase formed during HPT.

Deformation and failure behavior of nanocrystalline WCu

The technical potential of WCu alloys is limited by the modest fracture characteristics of the material system in its coarse-grained condition. To provide a nanocrystalline microstructure and improve mechanical properties, a W-50 at.% Cu composite was processed using high-pressure torsion deformation at a temperature of 200 °C. Therefore, two specimens were subjected to 100% and 1000% shear strains, respectively. Scanning electron and scanning transmission electron microscopy, including nanoscale energy dispersive X-ray spectroscopy mappings, were used to quantify the resulting microstructures. The average grain sizes for the 100% and 1000% deformed specimens were determined to be 14.7 ± 6.6 nm and 10.5 ± 5.6 nm, with the amount of mechanically intermixed W in the Cu grains increasing from 15.4 at.% to 15.9 at.%. X-ray diffraction and selected area electron diffraction studies both revealed strained lattice parameters of the W and Cu phases, respectively. Mechanical properties were investigated using in-situ notched microcantilever tests. The mean conditional fracture toughness and J-integral values were comparable for both conditions, at 3.7 ± 0.4 MPa√m and 245 ± 58 J/m2, respectively. The related behavior could be attributed to the low fault tolerance of the highly deformed states and was substantiated by cleaved globular W grains along the fractured surfaces. In addition, the detailed relationship between the altered grain boundary conditions, the degree of mechanical intermixing and the influence of the different microstructures on the fracture properties were carefully evaluated and discussed to pave the way for future application of these high-strength nanocomposites.

EFFECT OF HIGH PRESSURE TORSION ON STRUCTURE AND MECHANICAL PROPERTIES OF Al–Ca–Cu ALLOY

To improve the balance of strength and ductility of the Al–6% Ca–8% Cu (wt %) alloy, the high-pressure torsion (HPT) deformation followed by annealing was applied. The structure of the as-cast alloy consisted mainly of two eutectics [(Al) + AlCaCu] and [(Al) + (Al, Cu)4Ca + AlCaCu]. HPT through three turns leads to the formation of a predominantly submicrocrystalline structure, refinement of eutectic particles and their more uniform distribution in the sample volume, calcium segregation from AlCuCa and (Al, Cu)4Ca particles, and supersaturation of the (Al) solid solution with copper. Such a structure provides a strengthening of the alloy by a factor of 3.5, but contributes to its embrittlement. Subsequent annealing at 400°C achieves a good balance of strength and ductility of the alloy.

The key role of grain boundary state in deformation-induced softening effect in Al processed by high pressure torsion

The influence of type and amount of additional severe plastic deformation (SPD) on the magnitude of the deformation-induced softening (DIS) effect in ultrafine-grained (UFG) aluminum processed by high-pressure torsion (HPT) has been studied for the first time. Drastic DIS effect (the increase of plasticity from ∼1% to ∼23%), while maintaining high strength (ultimate tensile strength ∼ 180 MPa) is observed after a small additional deformation by HPT to 0.25 turns in UFG aluminum annealed at 150 °C for 1 h. An increase of additional HPT deformation to 0.75 turns does not lead to an increase of the DIS effect. The change of the type of additional deformation from HPT to cold rolling does not lead to any DIS effect, but slight hardening occurs and plasticity remains at low level (1–3%). The analysis of the evolution of the microstructure in correlation with mechanical behavior after annealing and subsequent deformations of both types indicates the key role of the state of the grain boundaries for the DIS effect in pure aluminum processed by HPT.

Exceptional strength-plasticity synergy in β-Ti alloy via HPT and short-period annealing

A new metastable β-type Ti-3.5Al-5Mo-4 V (Ti-B20) alloy with a high strength has been recently developed. However, the plasticity of the alloy after solution or aging treatment is poor due to its large initial β grain size, and conventional deformation-induced grain refinement is quite limited. In the present work, a high-pressure torsion (HPT) method was used to manufacture a Ti-B20 alloy with large deformed grains. The Ti-B20 alloy subjected to HPT was annealed in a β-phase field (850 ℃) for different periods. The deformation mechanism during HPT processing and the recrystallization behavior of the deformed alloy were systematically revealed. The results show that the deformation mode during HPT processing is mainly dislocation slip and shear band splitting of the original grains and martensitic phase (α″). During recrystallization annealing, the shear bands and high-density dislocations generated by the HPT deformation of the Ti-B20 alloy significantly promote nucleation and growth of recrystallized grains, which shortens the time to complete recrystallization. After recrystallization annealing, exceptional strength-ductility synergy with a high tensile strength of 941.9 MPa and a high plasticity of 39.7% is achieved in the fine-grained (14.68 µm) alloy, which is the highest elongation reported in the Ti-B20 alloy at present. The fine grains with a low dislocation density provide more space for dislocation slip and accumulation while maintaining high strength. This work provides a new possibility for preparing fine-grained β-titanium alloys with synergistic strength and plasticity.

Exchange Bias Demonstrated in Bulk Nanocomposites Processed by High-Pressure Torsion.

Ferromagnetic (Fe or Fe20Ni80) and antiferromagnetic (NiO) phases were deformed by high-pressure torsion, a severe plastic deformation technique, to manufacture bulk-sized nanocomposites and demonstrate an exchange bias, which has been reported predominantly for bilayer thin films. High-pressure torsion deformation at elevated temperatures proved to be the key to obtaining homogeneous bulk nanocomposites. X-ray diffraction investigations detected nanocrystallinity of the ferromagnetic and antiferromagnetic phases. Furthermore, an additional phase was identified by X-ray diffraction, which formed during deformation at elevated temperatures through the reduction of NiO by Fe. Depending on the initial powder composition of Fe50NiO50 or Fe10Ni40NiO50 the new phase was magnetite or maghemite, respectively. Magnetometry measurements demonstrated an exchange bias in high-pressure torsion-processed bulk nanocomposites. Additionally, the tailoring of magnetic parameters was demonstrated by the application of different strains or post-process annealing. A correlation between the amount of applied strain and exchange bias was found. The increase of exchange bias through applied strain was related to the microstructural refinement of the nanocomposite. The nanocrystalline maghemite was considered to have a crucial impact on the observed changes of exchange bias through applied strain.

Gripping Prospective of Non-Shear Flows under High-Pressure Torsion.

The article presents a theoretical study of the regimes of high-pressure torsion (HPT) for which slippage of the deforming material on the interfaces with anvils is possible. The approach taken is a generalisation of the currently accepted view of the HPT process. It enables a rational explanation of its salient features and the effects observed experimentally. These include a lag in the rotation angle of the specimen behind that of the anvils, an outflow of the material from the deformation zone, enhancement in gripping the specimen with anvils with increasing axial pressure, etc. A generalised condition for gripping the specimen with anvils, providing a basis for an analytical investigation of the HPT deformation at a qualitative level, is established. The results of the analytical modelling are supported by finite-element calculations. It is shown that for friction stress below the shear stress of the specimen material (i.e., for the friction factor m < 1), plastic deformation is furnished by non-shear flows, which expands the range of possible process regimes. The potential of these flow modes is impressive, which is reflected in the second meaning of the word “gripping” in the title of the article. Non-shear flows manifest themselves in the spreading of the material over the anvil surfaces whose cessation signifies the end of deformation and the beginning of slippage of the specimen as a whole. The model shows that for m < 1 such a finale is inevitable at any axial pressure. It predicts, however, that the highest achievable strain is increased when the axial pressure is raised in the course of the HPT process. Unlimited deformation of the specimen is only possible for m = 1, when slippage of the deforming material relative to the anvils is suppressed.

Temperature-Rate Conditions of Deformation&#x0D; and Structure-Forming Processes in Nickel&#x0D; during High-Pressure Torsion

Scanning and transmission electron microscopy has been used to investigate the nickel structure formed by high pressure torsion deformation at temperatures of 100–250°C. The relationship between the structure and temperature–rate conditions of deformation, which is characterized by the Zener–Hollomon parameter (Z), has been found. A change in the temperature–rate conditions of deformation has been shown to alter the dominant structure-forming process and to change the resultant structure. We have identified lnZ ranges where these processes occurred, namely, dynamic recovery at lnZ 25, dynamic recrystallization at 21 lnZ 25, and dynamic polygonization at lnZ 21.

Distribution of Order Parameter in Solids under High Pressure Torsion.

Severe plastic deformation (SPD) can lead to various phase transformations. High-pressure torsion (HPT) is one of the most important variants of SPD. In principle, HPT can continue almost indefinitely long, as long as the plungers are not destroyed. However, the number of defects in a material during HPT deformation cannot increase indefinitely. When the rate of defects production becomes equal to the rate of their annihilation, a steady state or dynamic equilibrium is reached. Unexplored is the issue of establishing equilibrium at the initial stage of plunger torsion, when there is an angular acceleration. The parameters of the steady state are described here using the idea of an order parameter in solids in the framework of Landau phenomenological theory and the Landau–Khalatnikov equation.

Thermal, Microstructural and Electrochemical Hydriding Performance of a Mg65Ni20Cu5Y10 Metallic Glass Catalyzed by CNT and Processed by High-Pressure Torsion

A Mg65Ni20Cu5Y10 metallic glass was produced by melt spinning and was mixed with a 5 wt.% multiwall carbon nanotube additive in a high-energy ball mill. Subsequently, the composite mixture was exposed to high-pressure torsion deformation with different torsion numbers. Complimentary XRD and DSC experiments confirmed the exceptional structural and thermal stability of the amorphous phase against severe plastic deformation. Combined high-resolution transmission electron microscopy observations and fast Fourier transform analysis revealed deformation-induced Mg2Ni nanocrystals, together with the structural and morphological stability of the nanotubes. The electrochemical hydrogen discharge capacity of the severely deformed pure metallic glass was substantially lower than that of samples with the nanotube additive for several cycles. It was also established that the most deformed sample containing nanotubes exhibited a drastic breakdown in the electrochemical capacity after eight cycles.

Formation and Thermal Stability of the ω-Phase in Ti-Nb and Ti-Mo Alloys Subjected to HPT.

This paper discusses the features of ω-phase formation and its thermal stability depending on the phase composition, alloying element and the grain size of the initial microstructure of Ti–Nb and Ti–Mo alloys subjected to high-pressure torsion (HPT) deformation. In the case of two-phase Ti–3wt.% Nb and Ti–20wt.% Nb alloys with different volume fractions of α- and β-phases, a complete β→ω phase transformation and partial α→ω transformation were found. The dependence of the α→ω transformation on the concentration of the alloying element was determined: the greater content of Nb in the α-phase, the lower the amount of ω-phase that was formed from it. In the case of single-phase Ti–Mo alloys, it was found that the amount of ω-phase formed from the coarse-grained β-phase of the Ti–18wt.% Mo alloy was less than the amount of the ω-phase formed from the fine α′-martensite of the Ti–2wt.% Mo alloy. This was despite the fact that the ω-phase is easier to form from the β-phase than from the α- or α′-phase. It is possible that the grain size of the microstructure also affected the phase transformation, namely, the fine martensitic plates more easily gain deformation and overcome the critical shear stresses necessary for the phase transformation. It was also found that the thermal stability of the ω-phase in the Ti–Nb and Ti–Mo alloys increased with the increasing concentration of Nb or Mo.

Grain Refinement in High-Entropy Alloys by High-Pressure Torsion Deformation

Grain Refinement in High-Entropy Alloys by High-Pressure Torsion Deformation

Annealing-induced recrystallization of iron after high pressure torsion at 80 K

Grain growth during recrystallization of pure iron with a submicrocrystalline structure formed by 5 revolutions of an anvil of high-pressure torsion deformation at cryogenic temperature (80 К) has been studied by transmission and scanning electron microscopy and durometry. Annealing at 523 К has significantly developed recrystallization (to 90 % of the material volume). The average recrystallized grain size is 2 μm. The primary recrystallization has been completed after 1‑h annealing at 823 К, forming grains with an average grain size of 6.5 μm. Annealing at 823 К has resulted in a large number of fine grains due to the formation of thermally activated centers of recrystallization. The grain size variability, which is characterized by the formation of grains with a size of five or more times greater than the average grain size, is observed. The average grain size has remained unchanged according to the scanning electron microscopy data, and decreased according to transmission electron microscopy data. The recrystallization texture of an axial <110> type has formed during annealing at 823 К. An increase in the annealing temperature to 923 К has increased the sharpness of the recrystallization texture. The hardness of iron has remained dependent on the true strain (distance from the sample center) after annealing at all temperatures under study.

Grain refinement and enhanced diffusion of W[sbnd]Cu gradient material processed by high pressure torsion with floating cavity

High-pressure torsion (HPT)processing with floating cavity was carried out under the applied pressure of 1.5 GPa with the revolution from 5 to 20 turns at the temperature of 300 °C, and the WCu gradient material with noble bonding interface and significant grain refinement was successfully obtained. The microstructure evolution and atomic diffusion around the bonding interface were analyzed by electron backscatter diffraction (EBSD), transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS) in a field emission scanning electron microscope (SEM). The mechanism of large shear strain on the microstructure evolution and diffusion ability of tungsten and copper at the interface was investigated. The results show that HPT processing with floating cavity can effectively refine microstructure of tungsten and copper to submicron. After 5 turns of HPT deformation, the grain size of copper was significantly refined to 0.59 μm but experiences slight increases to 0.8 μm with the additional revolution number to 20 turns, and the ultrafine equiaxed grains with relatively straight grain boundaries and few dislocations within grains were formed under the continuous dynamic recrystallization mechanism. However, the microstructure of tungsten was continuously refined within 20 turns of HPT processing due to the accumulation shear deformation, and a lamellar microstructure was formed along the WCu bonding interface with a gradient distribution in the width of banded grains from 0.06 μm at the interface to 0.33 μm towards the tungsten matrix. In addition, with the increase of torsion strain, the diffusion lengths of tungsten and copper gradually increasing to 1.6 μm and 6.2 μm, the interdiffusion coefficient of tungsten in copper remained basically constant, while the value of copper in tungsten increases continuously. The high density of defects and ultrafine grains with high angle boundaries introduced by large shear deformation of 20 turns of HPT processing play roles in the rapid diffusion paths to accelerate the atom diffusion and the interdiffusion coefficient of tungsten and copper is enhanced by 0.48– 1.79× 108 times compared to the lattice diffusion.

Achieving excellent mechanical properties in type 316 stainless steel by tailoring grain size in homogeneously recovered or recrystallized nanostructures

One hopeful path to realize good comprehensive mechanical properties in metallic materials is to accomplish homogeneous nanocrystalline (NC) or ultrafine grained (UFG) structure with low dislocation density. In this work, high pressure torsion deformation followed by appropriate annealing was performed on 316 stainless steel (SS). For the first time, we successfully obtained NC/UFG 316 SS having uniform microstructures with various average grain sizes ranging from 46 nm to 2.54 μm and low dislocation densities. Dislocation scarcity in NC/UFG grains was found bringing significant extra enhancement in strength in addition to normal grain boundary hardening, which provided great freedom in tailoring mechanical property of the material with the wide range of average grain sizes. Among the series, an unprecedentedly high yield strength (2.34 GPa) was achieved at the smallest grain size of 46 nm, in which dislocation scarcity induced hardening accounting for 57% of the strength. On the other hand, exceptional strength-ductility synergy with high yield strength (900 MPa) and large uniform elongation (27%) was obtained in the fully recrystallized specimen having the grain size of 0.38 μm, the finest recrystallized grain size ever reported. The high yield stress and scarcity of dislocation sources in recrystallized UFGs activated stacking faults and deformation twins nucleating from grain boundaries during straining, and their interaction with dislocations allowed for sustainable strain hardening, which also agreed with the plaston concept recently proposed. The multiple deformation modes activated, together with the effective strengthening mechanisms, were responsible for the outstanding comprehensive mechanical performance of the material.