High-pressure Torsion Processing Research Articles

Nanostructured bulk HPT β Ti-42Nb alloy as biomaterial for implants obtained directly from micrometric powders

The effect of high-pressure torsion (HPT) processing on mechanical properties in a β Ti-42Nb alloy micrometric powder consolidated in a nanostructured bulk disc through severe plastic deformation for biomedical applications is investigated. XRD, SEM and TEM/ASTAR characterization are used to characterize microstructure of the original micrometric powder and the consolidated disc of β Ti-42Nb alloy after HPT. The results show that severe plastic deformation processing improves Vickers hardness of β Ti-42Nb alloy, and leads to a low modulus bulk material with E = 63 GPa after HPT, comparable with that of as-cast alloy. The obtaining of nanostructured grain size around 55 nm bulk β Ti-42Nb alloy consolidated through HPT from micrometric atomized powder opens perspectives of applications as biomedical implants.

Ferromagnetism in High Entropy Cantor alloy triggered and tuned by severe plastic deformation

The process of severe plastic deformation (SPD) introduces unique conditions to materials, leading to the emergence of novel properties. This research specifically investigates the observation of deformation-induced ferromagnetism resulting from SPD processing. High-pressure torsion (HPT) is utilized to process both single-phase and nanocomposite high entropy alloys (HEAs). Vibrating sample magnetometry (VSM) confirms that HPT processing triggers the development of ferromagnetic properties. The distribution and alignment of magnetic domains post-SPD treatment are further examined using differential phase contrast scanning transmission electron microscopy (DPC STEM). Atom probe tomography (APT) analysis suggests that this phenomenon stems from the localized enrichment of ferromagnetic elements, particularly Ni, induced by deformation. This observation underscores the ‘cocktail effect’ in HEAs, whereby interactions between different elements has led to this unique magnetic behavior. Additionally, deliberate mechanical mixing of the CoCrFeMnNi alloy with a HfNbTaTiZr HEA, comprising non-ferromagnetic constituents, introduces a large rotational strain that alters the ferromagnetic properties. This mixing facilitates a transition from a random orientation of magnetic domains, as seen in the HPT-processed single CoCrFeMnNi alloy, to a coordinated alignment within the nanocomposite HEA.

Ultra-High Strength in FCC+BCC High-Entropy Alloy via Different Gradual Morphology.

In this study, high-pressure torsion (HPT) processing is applied to the as-cast Al0.5CoCrFeNi high-entropy alloy (HEA) for 1, 3, and 5 turns. Microstructural observations reveal a significant refinement of the second phase after HPT processing. This refinement effect is influenced by the number of processing turns and the distance of the processing position from the center. As the number of processing turns or the distance of the processing position from the center increases, the fragmentation effect on the second phase becomes more pronounced. The hardness of the alloy is greatly enhanced after HPT processing, but there is an upper limit to this enhancement. After increasing the number of processing turns to 5, the increase in hardness at the edge becomes less significant, while the overall hardness becomes more uniform. Additionally, the strength of the processed alloy is significantly enhanced, while its ductility undergoes a noticeable decrease. With an increase in the number of processing turns, the second phase is further refined, resulting in improvement of strength and ductility.

Effect of High-Pressure Torsion Temperatures on the Precipitation and Properties of Cu-Cr Alloy.

This study examines the impact of high-pressure torsion (HPT) processing at various temperatures on the precipitation behavior of Cu-Cr alloys. The introduction of defects through HPT is observed to promote the precipitation of Cr atoms. Unlike the traditional large-scale precipitation that typically occurs around 400 °C, HPT can induce the precipitation of solute atoms even at room temperature. Furthermore, the temperature at which HPT is performed significantly influences the behavior of the precipitated phase during subsequent aging, ultimately affecting the alloy's overall properties. At elevated temperatures (ETs) and room temperature (RT), Cr atoms tend to aggregate, forming Guinier-Preston (GP) zones or precipitates, which coarsen into incoherent precipitates after annealing. In contrast, when HPT is conducted at liquid nitrogen temperature (LNT), Cr atoms are retained in their original positions, leading to the formation of uniformly distributed, high-density small precipitates post-annealing. This phenomenon results in superior properties for HPT-LNT-treated samples, evidenced by a microhardness of 191.8 ± 3.2 HV and an electrical conductivity of 84.6 ± 1.8% IACS.

Optimizing the mechanical and corrosion properties of an ultrafine-grained Al-Cu-Mg alloy through cyclic deformation: Clusters and lattice defects

To optimize its corrosion and mechanical properties, an Al-Cu-Mg alloy is cyclically processed by high-pressure torsion (HPT), involving a 1/2 turn clockwise and a 1/2 turn counter-clockwise per cycle. The dislocation density increases to 3.04×1014 m−2 on 1 cycle HPT and decreases gradually to 2.23×1014 m−2 for higher cyclic rotations (i.e. 5 cycle HPT). Due to the rapid elimination of the geometrically necessary dislocations, the refinement of grain size in cyclic HPT is more efficient than the monotonic HPT (i.e. it decreases from 2.48 μm to 112 nm on 1 cycle HPT). The HPT samples are electrochemically corroded in a simulated seawater environment. 1-cycle HPT process causes a strong increase in hardness (to 232 HV) and an increase in corrosion potential (to −0.517 V). The trade-off between hardness/strength and corrosion resistance is broken on cyclic HPT processing. Aided by excess vacancies induced by HPT, Cu-Mg clusters form on and near grain boundaries through a ‘vacancy-pump’ mechanism, causing solute depleted zones (SDZ) adjacent to GBs. The combined effects of ultrafine grains, solute cluster segregation and SDZs enhance the strength and corrosion resistance of the Al-Cu-Mg alloys. This study provides a potential strategy to design the microstructures of an Al alloy, and to achieve a higher hardness and a better corrosion performance of that material.

Effect of intermediate processing treatment on the structure and mechanical properties of Al–4 wt%Cu–3 wt%Mn alloy manufactured by electromagnetic casting followed by high-pressure torsion (HPT)

In this work, a thermally stable model Al–4Cu–3Mn (wt%) alloy has been manufactured by electromagnetic casting (EMC), followed by compression, intermediate heat treatment and high-pressure torsion (HPT). Structural changes of the alloy during subsequent processing stages have been analysed by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and the X-ray diffraction (XRD). The results indicate that variations in the intermediate heat treatment temperature of the compressed samples lead to a significant difference in strain hardening and thermal stability after HPT. According to microstructure investigations the hardening of samples processed by HPT resulted from formation of mixture of grains and subgrains with high dislocation density as well as mechanical fragmentation of eutectic Al2Cu particles and precipitation of nanoscale Mn-rich dispersoids which are identified as Al6Mn. The intermediate heat treatment of the EMC rod at 350 ºC for 3 hours and heat treatment of HPT sample at 250 ºC for 5 hours exhibited the best mechanical properties in terms of ultimate tensile strength (UTS), yield strength (YS) and elongation (El), reaching 610 MPa, 560 MPa and 10 % respectively. At the same time intermediate annealing at 450 °C makes the HPT processing ineffective.

Phase transformation and mechanical properties of nanocrystalline Ti–2Fe-0.1B alloy processed by high pressure torsion

In this paper, nano-Ti-2Fe-0.1B alloys with different grain sizes were processed by high pressure torsion (HPT) deformation. The study examined the microstructural evolution of the Ti–2Fe-0.1B alloy during HPT and evaluated its mechanical properties through microhardness and tensile tests. The results of the microstructural observations revealed that the grain size of the Ti–2Fe-0.1B alloy progressively decreased from 3.14 μm in the as-annealed state to approximately 20 nm after 10 turns. In the initial state, the alloy consists of α-phase and β-phases, with a volume ratio of approximately 5:1. During the HPT process, transformations of α-phase and β-phase to ω-phase were observed. The primary reason for this is that the shear forces applied during the HPT process facilitated the phase transformation of the α-phase. Additionally, the presence of Fe element in the alloy altered the lattice compatibility between the grains of β-phase and ω-phase, thereby promoting the phase transformation of the β-phase, with the accumulated turns of HPT process, the fraction of ω-phase increased in the beginning gradually, then decreased, which reached to the maximum 80.8% in the 5 turns. This is higher than that of pure titanium and Ti–Fe alloys under the same conditions, because the proportion of the ω-phase increases with the increase in Fe content. Studies of mechanical properties demonstrated that HPT can substantially enhance the hardness of Ti–2Fe-0.1B alloys to as high as 483 HV, and the tensile strength of the Ti–2Fe-0.1B alloy was observed to increase from 725 MPa to 1568 MPa after 5 turns, which is much higher than Ti–6Al–4V subjected to the identical processing conditions. It can be ascribed to the exist of mass ω-phase as well as finer grain size in nanocrystalline Ti–2Fe-0.1B alloy.

Fracture behaviour assessment of the additively manufactured and HPT-processed Al–Si–Cu alloy

Ultrafine-grained Al–9%Si–3%Cu alloy was achieved by a combination of laser powder bed fusion (LPBF) additive manufacturing and high-pressure torsion (HPT) processing in this investigation. The alloy was initially deposited layer-by-layer using a bi-directional scan strategy in LPBF with a scan rate of 1000 mms−1, a layer thickness of 40 µm and a hatch spacing of 200 µm, leading to a melt pool morphology with an average width of 150 µm and differing lengths. This led to a grain size of 722 nm and a dislocation density of 1.1 × 1014 m−2. This as-deposited alloy was then processed using HPT at room temperature using an applied pressure of 6.0 GPa and at a speed of one revolution per minute for different numbers of turns: half, one, five and ten turns. The alloy after HPT processing showed ultrafine grains with a grain size of 66 nm, well-dispersed nanosized intermetallic particles with sizes of 50–90 nm, the disappearance of the pool morphology and a notable dislocation density of about 6.2 × 1014 m−2 for the ten turns HPT-processed alloy. The as-deposited and subsequently HPT-processed samples were tensile tested at 298 and 573 K at different strain rates between 10−4 and 10−1 s−1. The elongation-to-failure and tensile strength were recorded and the fracture surfaces were also inspected using scanning electron microscopy and then correlated with the manufacturing, processing and tensile testing conditions. The alloy performance in tensile testing has been evaluated at ambient and elevated temperatures in terms of structural evolution and fractography for the first time. Ultrafine α-aluminium grains and nanosized eutectic silicon particles obtained by room temperature HPT-processing of the alloy have significantly improved the mechanical properties and microstructural stability at ambient and elevated testing temperatures for the HPT-processed additively manufactured alloy compared to the as-deposited additively manufactured and counterpart conventional alloys. The HPT-processed tensile samples showed a significant tensile strength of 700 MPa at 298 K and elongation-to-failure of 220% at 573 K, which is higher than that seen in the as-deposited tensile samples where 400 MPa and 106% are observed under the same testing conditions. Fractographic observations demonstrated that mixed brittle and shear ductile fractures dominated in the as-deposited tensile samples at 298 K, and tension ductile fracture dominated at 573 K. However, the HPT-processed tensile samples exhibited tension ductile and shear ductile fractures at 298 K, and tension ductile fracture at 573 K. The ultrafine-grained microstructure produced by the HPT application in the LBPF-manufactured alloy controls effectively the fracture mechanisms, dimple morphology and thus strength and elongation in comparison with the as-deposited additively manufactured microstructure.

High corrosion resistance of nanograined and nanotwinned Al0.1CoCrFeNi high-entropy alloy processed by high-pressure torsion

This study examines the corrosion resistance of ultrafine-grained Al0.1CoCrFeNi high-entropy alloy processed by high-pressure torsion (HPT), focusing on stored energy, diffusion, and the high-entropy effect. Microstructural analysis revealed a single-phase FCC structure with numerous defects and reduced crystallite size following the HPT process. Samples with higher HPT turns formed high-angle grain boundaries, equiaxed nanograins, and numerous nanotwins, contributing to a notable increase in Vickers microhardness from 159 Hv for the initial sample to 550 Hv after 5 turns of HPT. Corrosion behavior is found to be influenced by stored energy and chromium diffusion. Low HPT turns increased the corrosion rate due to sluggish diffusion of chromium and high stored energy in the form of dislocations. Conversely, corrosion resistance improved with increased HPT turns due to fast diffusion through non-equilibrium grain boundaries and the formation of nanotwins with lower stored energy. These findings suggest that a relatively low entropy plays a critical role in the chromium segregation from the solid solution for forming a passive film and enhancing corrosion resistance.

Microhardness and Microstructure of Aluminium Alloy 5052 by High-Pressure Torsion Process and Subsequent Annealing

The grain refinement by high-pressure torsion (HPT) process and high-temperature stability have been studied in a commercial non-heat-treated aluminium alloy, 5052. The HPT process was conducted on 10 mm disks of the alloys at room temperature with an applied pressure of 6 GPa for 5 and 10 turns with a rotation speed of 1 rpm. The HPT processing leads to microstructural refinement with an average grain size of ~188 nm and ~156 nm for 5 turns and 10 turns with an increased value of dislocation density. The Vickers microhardness test was performed at 100 gf for a duration of 15 s. It was found that the hardness increased from the onset of straining and saturated at approximately 165 Hv after processing at both 5 and 10 turns. The samples were then annealed at high temperatures. The study demonstrated that annealing at 200 °C for 1 h reduced the hardness by 30% in both samples and enlarged the gain sizes to 226 nm. The results indicated that the rate of hardness decrease is faster in 10 turns compared with 5 turns thus explaining the higher kinetic annihilation phenomenon observed in higher straining in 10 turns due to the higher stored energy in the grains.

Severe plastic deformation of two-phase TiNiCuNb shape memory alloy

(Ti54Ni34Cu12)90Nb10 alloy with initial two-phase structure of B19 martensite and β-Nb phase was subjected to high-pressure torsion (HPT) process at room temperature. HPT leads to the formation of nanocrystalline bands of β-Nb phase alternating with amorphous matrix. Nanocrystalline debris of B2 phase was found to be embedded into the amorphous matrix. Refinement of β-Nb phase upon HPT is much greater compared to that for pure Nb alloy.

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.

Nanostructuring of Additively Manufactured 316L Stainless Steel via High-Pressure Torsion for Enhanced Strength and Corrosion Performance

Bulk nanostructured materials (BNM) are defined as metallic materials with grain sizes &lt;100 nm and are known to possess superior mechanical and functional properties compared to those with grain sizes in the micron and millimeter ranges. In this study, high-pressure torsion (HPT), a nanostructuring approach that imposes compressive stress and extreme torsional strain on bulk materials is applied to an additively manufactured (AM) 316L stainless steel (316L SS) for 10 revolutions. The grain sizes, hardness, and corrosion performance before and after HPT are evaluated by using extensive microscopy techniques, Vickers hardness (HV) measurements, and electrochemical tests conducted in 3.5 wt.% NaCl solution, respectively. The results show that after 10 HPT revolutions, nano-sized grains (average: ~42 nm) are obtained, whereas a three-fold increase in HV values from ~220 HV to ~600 HV are observed. Furthermore, the corrosion performance is also significantly enhanced as indicated by the reduction in corrosion ratefrom 2.53 μm/year initially, to 0.48 μm/year after HPT processing. These results highlight the benefits of HPT in producing bulk nanostructured materials with remarkably high hardness and excellent corrosion performance, potentially useful for a myriad of applications.

High‐Pressure Torsion Processing of Serine and Glutamic Acid: Understanding Mechanochemical Behavior of Amino Acids under Astronomical Impacts

Astronomical impacts by small solar system bodies (meteoroids, asteroids, comets, and transitional objects) are considered a mechanism for delivering amino acids and their polymerization to proteins in early Earth conditions. High‐pressure torsion (HPT) is a new methodology to simulate such impacts and clarify the behavior of biomolecules. Herein, two amino acids, crystalline L‐serine and L‐glutamic acid that are detected in meteorites, are processed by HPT and examined by ex situ X‐ray diffraction, Raman spectroscopy, nuclear magnetic resonance, Fourier‐transform infrared spectroscopy, and in situ mechanical shear testing. No polymerization, chemical reactions, or phase transformations are detected after HPT, indicating that the stability and presence of these two amino acids in meteorites are quite reasonable. However, some microstructural and mechanical changes like crystal size reduction to the nanometer level, crystal defect formation, lattice expansion by vacancy formation, and shear strength enhancement to the steady state are found which are similar to the behaviors reported in metals and ceramics after HPT processing.

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.

High-pressure-torsion-induced segregation, precipitation and grain refinement of Al-(Si, Mg and Cu) binary alloys

To uncover the effects of segregation and precipitation on grain refinement of metals under severe plastic deformation, high-pressure-torsion (HPT) processing is performed on three binary Al-(Si, Mg, and Cu) alloys with different stability and segregation characteristics. Atom probe tomography analysis reveals that HPT processing induces significant decomposition of Al-1 at% Si and Al-1 at% Cu alloys with coarse Si particles and fine Al2Cu (θ) precipitates formed, but no decomposition of Al-1 at% Mg alloy, with dislocations segregated with Si, Cu, and Mg, and grain boundaries (GBs) only segregated with Cu and Mg. The GB segregation of Cu is stronger than that of Mg and Si, with Cu excess in the range of 1.5–7.0 atoms/nm2, Mg excess in the range of 0–4.0 atoms/nm2, but no Si excess. Interestingly, some GBs without Mg segregation develop a Mg-depletion zone along a single side. All evidences demonstrate that GB segregation and precipitation are responsible for HPT-induced grain refinement of Al-1Mg and Al-1Cu alloys but coarsening of the Al-1Si alloy. Engineering solute distribution is of significance in controlling the ultrafine grain of the Al alloys.

Crystal-to-amorphous phase transformation in ternary shape memory alloys

This systematic study evaluates the role of important factors in crystal-to-amorphous phase transformation during severe plastic deformation in ternary shape memory alloys. Experiments coupled with thermodynamic calculations to obtain comprehensive interpretation on the amorphization in ternary shape memory alloys. Equiatomic binary NiTi together with ternary Ni–45Ti–5Hf and Ti–45Ni–5Cu (at%) alloys as alloy models were processed by high-pressure torsion (HPT) at room and cryogenic temperatures. The binary and Hf-added alloys revealed an amorphous structure with a few remaining nanocrystals, however, Cu-added ternary alloy showed resistance to the amorphization after HPT processing. The results revealed two key factors of preventing martensite-to-austenite transformation during deformation and the intrinsic potential of the material for amorphization drive crystal-to-amorphous phase transformation. Higher transformation temperatures, enthalpy and thermal hysteresis prevented martensite-to-austenite transformation, which therefore encouraged amorphization. In addition, a large negative heat of mixing, Gibbs energy for amorphization and a large atomic size mismatch are important factors in implementing crystal-to-amorphous phase transformation. This investigation is a step forward to a fundamental understanding of ternary or even compositionally complex shape memory alloys for microstructural engineering by providing a homogeneous ultrafine-grained structure due to amorphization and subsequent heat treatment to achieve superior shape memory effect and superelasticity.

Surface sliding revealed by operando monitoring of high-pressure torsion by acoustic emission

High-pressure torsion (HPT) is widely used as a key method for microstructure control through deformation processing across a broad range of materials. However, certain gaps in process control impact its efficacy. In this study, we investigate the acoustic emission (AE) signals generated during HPT by considering commercially pure molybdenum as an example. By employing the adaptive sequential k-means algorithm, we analyse the AE stream to categorise and identify its sources. By comparing the kinetics of AE signal evolution during HPT processing at pressures of 2 GPa and 5 GPa, two distinct signal types are identified: one linked to plastic deformation and the other to workpiece slippage over HPT anvil surfaces. This research demonstrates the potential of AE tools for operando monitoring of HPT stability and detection of workpiece slippage, thereby enhancing the processing efficiency.

Enhanced Microhardness and Corrosion Performance of Additively Manufactured Inconel 718 Specimens through Nanostructuring by Severe Plastic Deformation

Severe plastic deformation (SPD) processes, particularly high-pressure torsion (HPT) have been increasingly applied to metallic specimens fabricated by laser powder bed fusion (L-PBF) additive manufacturing (AM) for enhancing their mechanical and functional properties through nanoscale grain refinement (≤ 100 nm). In this study. L-PBF AM-fabricated Inconel 718 (IN 718) specimens are initially subjected to 10 HPT revolutions to produce nanosized grains. Subsequently, microstructural characterisation, as well as hardness and electrochemical tests are conducted to evaluate the evolution of microstructures, hardness, and corrosion performance of the as-received and HPT-processed specimens by using various microscopy, Vickers microhardness (HV) measurements, and corrosion performance, respectively. The results reveal an average grain size of ~ 46 nm, dense dislocation networks, and nanotwins after 10 HPT processing, which contribute to the two-fold hardness increase compared to the as-received condition. Such microstructures also contributed to the overall improved corrosion performance after 10 HPT processing, as quantified by the 83% and 73% reduction in corrosion rate and pitting potential, respectively.

Evaluating High‐Pressure Torsion Scale‐Up

Increasing sample dimensions in high‐pressure torsion (HPT) processing affects load and torque requirements, deformation distribution, and heating. Finite‐element modeling (FEM) and experiments are used to investigate the effect of technical parameters on the scaling up of HPT. Simulations confirm that axial load and torque requirements are proportional to the square and the cube of the sample radius, respectively. The temperature rise also displays a pronounced dependency on the radius. Decreasing the diameter‐to‐thickness ratio can cause heterogeneity in strain distribution along the thickness direction at the edges of the sample. Such heterogeneity is governed by friction conditions between the material and the lateral wall of the anvil depression. Simulation of HPT processing of ring‐shaped samples shows that it is possible to reach more homogeneous distribution of strain and flow stress in the processed material. Experiments using magnesium confirm a tendency for strain localization in the early stage of HPT processing but increasing the number of turns increases the homogeneity of the material. The embodied energy in HPT processing is discussed.