Ultrafine-grained Ti Research Articles

Microstructure and Mechanical Properties of Titanium Alloys Produced by Additive Technologies: New Approaches and Promising Areas of Research

Additive manufacturing, or 3D printing, is a process where a part is produced layer by layer, and represents a promising approach for designing components close to their final shape. Titanium alloys produced by additive manufacturing find application in various industries. This overview examines the features of the formation of the microstructure and properties in Ti alloys synthesized with the use of powder and wire laser additive technologies, as well as solid-phase methods of additive manufacturing such as friction stir additive manufacturing. Their main drawbacks and advantages are discussed, as applied to Ti alloys. The main approaches to solving the problem of increasing the strength properties of the synthesized Ti workpieces are considered. The authors of this overview propose a new area of research in the field of the application of additive technologies for producing ultrafine-grained Ti semi-products and parts with enhanced performance characteristics. Research in this area opens up prospects for designing heavily loaded complex-profile products for the aerospace, oil and gas, and biomedical industries.

Microstructural modification and mechanical improvement of ultrafine-grained Ti alloy through electron wind force: An innovative approach

This study focuses on the effect of high-density pulsed electric current (HDPEC) on the microstructure and mechanical properties of ultrafine-grained (UFG) Ti–6Al–7Nb (mass%) alloy. After the UFG Ti alloy prepared by high-pressure torsion (HPT), the samples exhibit high tensile yield strengths of 1200 MPa with total elongation of ∼20 %. Interestingly, an unusual improved elongation of ∼33 % with a yield strength of 1100 MPa was obtained in samples processed by HPT plus HDPEC. Quantitative evaluation shows that the improved ductility is attributed to the decreasing of dislocation density. The electron wind force played an important role to promote the movement of dislocation easier with the assistance of local Joule heating during HDPEC processing. It is shown that the bimodal structure with a low dislocation density leads to the high strength and high ductility. It indicated that HDPEC give an effective method to improve the ductility in UFG alloys.

Comparative evaluation of osseointegration of new percutaneous implants made of Ti Grade 4 ultrafine‑grained alloy

Introduction It has been shown that titanium implants with a structured surface provide an increased rate of osseointegration what makes their application quite promising.The purpose of this work was to conduct a comparative evaluation of the efficiency of osseointegration of new percutaneous implants for prosthetics made of ultrafine-grained Ti Grade 4 alloy.Materials and methods The study was carried out on 12 male rabbits of the Soviet Chinchilla breed. Six rabbits of the control group had implants made of Ti6Al4V powder using selective laser sintering technology that were osseointegrated into the tibia, 6 rabbits of the experimental group had implants made of Ti Grade 4 by equal channel angular pressing. The formation of the "bone-implant" block was examined 26 weeks after the implantation.Results Histologically, after 26 weeks of the experiment, porous changes, enlargement of the Haversian canals, and pronounced osteoclastic resorption were not detected in the animals of the experimental group throughout the stump in the compact plate. Around the implant, a bony case repeating the bone shape was formed, represented by lamellar bone tissue. Using X-ray electron probe microanalysis, it was found that in the substrate formed on the surface of the implant in rabbits of the experimental group, there was significantly more calcium in all areas over the implant relative to the animals of the control group. In the control group, relative to the experimental group, an increased level of C-reactive protein in blood serum was retained longer. Complications and significant clinical and laboratory abnormalities were not found in both groups during the entire experiment.Discussion Our data are consistent with the results of other experimental studies, which unambiguously noted that titanium implants with a structured surface show increased osseointegration characteristics in comparative studies relative to implants without modification of the structure of the material of the threaded surface. The absence of complications and undesirable reactions of the animal organism also indicates the acceptable safety of the tested products.Conclusion Osseointegration of a percutaneous implant that has a mixed nanocrystalline and ultrafine-grained structure was more effective than the reference implant. This makes the use of such implant promising for solving clinical problems in prosthetics.

Thermal Properties, Energy Dissipation, and Storage During Deformation of Ultrafine Grained Ti-, Zr-, Nb-, and Mg-Based Alloys

Thermal Properties, Energy Dissipation, and Storage During Deformation of Ultrafine Grained Ti-, Zr-, Nb-, and Mg-Based Alloys

The Effect of Microstructural Defects on High-Cycle Fatigue of Ti Grade 2 Manufactured by PBF-LB and Hydrostatic Extrusion

The aim of this study was to show the effect of manufacturing defects in a commercially pure Ti Grade 2 produced by a laser beam powder bed fusion (PBF-LB) process on its high-cycle fatigue life. For this purpose, the high-cycle fatigue performance of PBF-LB Ti Grade 2 was compared to its ultrafine-grained (UFG) counterpart processed by hydrostatic extrusion exhibiting a similar mechanical properties under static tensile. The yield strength of the PBF-LB and UFG Ti Grade 2 was 740 and 783 MPa, respectively. The PBF-LB Ti Grade 2 consisted of a typical columnar of prior β grains with an acicular martensite α’ microstructure, while UFG Ti Grade 2 was mainly composed of fine, equiaxed α phase grains/subgrains with a size of 50–150 nm. A residual porosity of 0.21% was observed in the PBF-LB Ti Grade 2 by X-ray computed tomography, and, despite similar yield strength, a significantly higher endurance fatigue limit was noticed for UFG Ti Grade 2 (420 MPa) compared to PBF-LB Ti Grade 2 (330 MPa). Fatigue striation analysis showed that the fatigue crack propagation rate was not affected by manufacturing technology. In turn, the high-cycle fatigue life was drastically reduced as the size of manufacturing defects (such as pores or lack of fusion zones) increased.

The influence of microstructure and texture on the hardening by annealing effect in cold-rolled titanium

The purpose of this study was to compare the influence of microstructural and textural changes on the hardening by annealing effect in cold-rolled titanium. Ultrafine-grained (UFG) Ti Grade 2 was produced by multi-pass cold rolling (or warm rolling at 400 °C at the final stage) to different thickness reductions (90%, 95% and 97%) aimed at varying both the microstructural features of the material (dislocation density, grain size distribution and grain boundary characteristics) and its texture (the intensity and volume fraction of texture components). The hardening effect of UFG Ti Grade 2 sheets was obtained by a short-time annealing at 250 °C for 15 min. The highest strengthening, of about 4–5%, was observed for the UFG Ti Grade 2 sheet rolled to 90%; the strengthening gradually decreased for higher thickness reductions (down to ∼ 2% for 97%). The texture intensity and volume fractions of texture components for the annealed UFG Ti Grade 2 sheets were very close to their as-rolled counterparts, so this did not demonstrate any clear reason for the hardening effect. Instead, the dislocation substructure recovered during annealing at 250 °C, i.e. the dislocation density declined significantly, the remaining dislocations became rearranged, and it was easier to differentiate more nanosized subgrains of about 50–150 nm. The hardening by annealing effect was a result of the annihilation of mobile dislocations and the ordering of the dislocation substructure, mostly within coarse grains (>500 nm). The level of strengthening by low-temperature annealing was mainly affected by the fraction of coarse grains with a tangled-dislocation substructure in the as-rolled state, i.e. a higher fraction of coarse grains favored more pronounced strengthening. These observations seem to be very promising for optimizing the cold rolling process and short-time annealing of the UFG Ti Grade 2 sheets, which could be a simple and cost-effective way of enhancing their mechanical properties.

Thermal Stability and Mechanical Behavior of Ultrafine-Grained Titanium with Different Impurity Content

Ultrafine-grained (UFG) commercially pure (Ti Grade 2) and high-purity (Ti 99.99%) titanium can be a good alternative to less biocompatible Ti alloys in many biomedical applications. Their severe plastic deformation may lead to a substantial increase of strength, but their highly refined microstructure show a lower thermal stability which may limit their range of applications. The purpose of this study was to investigate the effect of interstitial elements on the thermal stability of UFG Ti Grade 2 and high-purity Ti 99.99% processed by a multi-pass cold rolling to the total thickness reduction of 90%. The severely cold rolled Ti sheets were annealed at temperature in the range of 100-600 °C for 1 h and, subsequently, they were evaluated in terms of microstructure stability, mechanical performance as well as heat effects measured by differential scanning calorimetry (DSC). It was found that the microstructure and mechanical properties were relatively stable up to 200 and 400 °C in the case of UFG Ti 99.99% and Ti Grade 2, respectively. DSC measurements confirmed the aforementioned results about lower temperature of recovery and recrystallization processes in the high-purity titanium. Surprisingly, the discontinuous yielding phenomenon occurred in both investigated materials after annealing above their thermal stability range, which was further discussed based on their microstructural characteristics. Additionally, the so-called hardening by annealing effect was observed within their thermal stability range (i.e., at 100-400 °C for UFG Ti Grade 2 and 100 °C for UFG Ti 99.99%).

Strength of Products Made of Ultrafine-Grained Titanium for Bone Osteosynthesis.

This paper evaluates the fatigue strength of ultrafine-grained (UFG) Grade 4 Ti in the low-cycle fatigue region, as well as the strength of medical implants (plates and screws) made of UFG Ti under various types of loading in comparison with the strength of products made of coarse-grained (CG) Ti. To produce a UFG state, titanium billets after annealing were processed by the ECAP-Conform technique. The fatigue of the prismatic specimens with a thickness of 10 mm from CG and UFG Ti was tested by the three-point bending method using an Instron 8802 facility. The modeling and evaluation of the stress-strain state in the ANSYS software package for finite-element analysis revealed, in particular, the localization of equivalent stresses in the area of hole edges and at fillets during the tension of the plates. The performed research has demonstrated that medical implants (plates and screws) from UFG Grade 4 Ti have a higher strength under different types of loading (tension, fatigue strength, torsion) in comparison with products from CG Ti. This opens up a possibility for the miniaturization of medical products from UFG Ti while preserving their main performance properties at an acceptable level.

Finite Element Modeling for Virtual Design to Miniaturize Medical Implants Manufactured of Nanostructured Titanium with Enhanced Mechanical Performance.

The study is aimed to virtually miniaturize medical implants produced of the biocompatible Ti with improved mechanical performance. The results on the simulation-driven design of medical implants fabricated of nanostructured commercially pure Ti with significantly enhanced mechanical properties are presented. The microstructure of initially coarse-grained Ti has been refined to ultrafine grain size by severe plastic deformation. The ultrafine-grained (UFG) Ti exhibits remarkably high static and cyclic strength, allowing to design new dental and surgical implants with miniaturized geometry. The possibilities to reduce the implant dimensions via virtual fatigue tests for the digital twins of two particular medical devices (a dental implant and a maxillofacial surgery plate) are explored with the help of finite element modeling. Additionally, the effect of variation in loading direction and the fixation methods for the tested implants are studied in order to investigate the sensitivity of the fatigue test results to the testing conditions. It is shown that the UFG materials are promising for the design of a new generation of medical products.

Finite element analysis of stress-strain state of the deformation zone of a UFG TI Grade 4 workpiece subjected to abrasive-free ultrasonic finishing

An effective approach to increasing the fatigue resistance of metal products is to create compressive residual stresses on the surface of the product using surface plastic deformation (SPD) processing. One of the effective SPD methods is the process of abrasive-free ultrasonic finishing (AFUF). Another well-known approach to improving mechanical properties including fatigue resistance is to create an ultrafinegrained (UFG) structural state in the product. This research focuses on the finite-element study of the stress-strain state of a UFG workpiece subjected to SPD by the AFUF method. Commercially pure Grade 4 titanium in the UFG state obtained by the ECAP-Conform method was chosen as a workpiece material. In the course of the study, the stress-strain state of the deformation zone was analyzed after a single indentation with subsequent unloading under the elastic-plastic scenario. The effect of the indenter oscillation amplitude and its geometry on radial residual stresses including their depth of occurrence, average normal stress and strain intensity was analyzed. It was found that as the indenter radius increases, the strain intensity (e) value decreases. The e parameter distribution has a gradient nature with a decrease in values from the surface to the center of the workpiece. An analysis of simulation results shows that radial residual stresses in the deformation zone are predominantly compressive, and, accordingly, they will increase the fatigue resistance of the finished product. It was established that as the indenter oscillation amplitude increases, the values of compressive radial residual stresses also increase. Their maximum values reach 540 MPa at an amplitude of 75 μm with the depth of these stresses up to 0.3 mm. An increase in the indenter radius, i.e. in fact the contact area, leads to an increase in the magnitude of compressive radial residual stresses with an almost linear behavior.

Micro-nano twins appearing in ultrafine-grained Ti–6Al–4 V alloy induced by high-pressure water jet technology

In this study, the surface of an ultrafine-grained Ti–6Al–4 V alloy was treated with high-pressure water jet technology (HPWJT). Then, the microstructure of the alloy was investigated using electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Three obviously different microstructural characteristics were observed from the treated surface to the matrix: ultrafine equiaxed grains with diameters from hundreds of nanometers to a few micrometers, micro-nano twins inside ultrafine equiaxed α grains, and an initial undeformed microstructure with ultrafine equiaxed grains. Formation of micro-nano twins in the subsurface was related to the special misorientation angle of neighboring grains. We proved the dependence of twinning on the crystallographic orientation and grain size of the α phase. In addition, the quantitative contributions of the micro-nano twins to the surface hardness of the alloy were calculated; micro-nano twins significantly improved the surface hardness of the alloy. This study provides a new easy method for introducing micro-nano twins on the surfaces of Ti and its alloys, and it may further improve the mechanical properties of these alloys.

The impact of severe plastic deformations obtained by hydrostatic extrusion on the machinability of ultrafine-grained Ti grade 2 intended for fasteners

The study aimed to examine the effect of the hydrostatic extrusion (HE) process on the machinability of Ti grade 2 (Ti) in the turning process. After the deformation with true strain ɛ = 2.28, the microstructure was significantly refined to a grain size of 100 nm, resulting in an increase in the mechanical properties, UTS strength by 190%, YS yield strength by 230%Cutting forces for Ti in the initial state and after HE were analyzed at cutting depths ap = 0.3 mm and 0.5 mm, the variables were cutting speed Vc (20, 30 and 50 m/min) and feed rate f (0.08 and 0.13 m/s).The impact of the microstructure refinement in Ti after HE on the high cutting depth machinability deterioration (ap = 0.7 mm) was identified. This phenomenon is particularly noticeable at lower cutting speeds Vc = 20 and 30 m/min at which cutting forces are higher. Application tests of Ti after HE showed a significantly lower susceptibility to buckling during threading. As a result of the tests carried out for the Ti in the initial state, it was not possible to achieve the tolerance of pitch diameter of the thread required by standards, d2 at two of the three cutting depths tested. In turn, for the Ti after HE, the thread tolerances required by the standards were achieved for all tested cutting depths.

Microstructure evolution and shear band formation in an ultrafine-grained Ti–6Al–4V alloy during cold compression

It is generally accepted that dynamic recrystallization (DRX) is the result of shear banding in metallic materials. However, we observed the microstructure evolution in an ultrafine-grained Ti–6Al–4V alloy under quasi-static compression and found the formation of DRX induced micro shear bands at the initial stage of plastic deformation. It is of interest that the strain-localized regions experienced a two-step recrystallization process, thus resulting in the formation of refined dynamic recrystallized (DRX) grains in transition zones and nanograins in core regions of micro shear bands successively. It is suggested that the DRX taking place at local regions led to the strain softening, which subsequently accelerated the formation of micro shear bands. Micro shear bands nucleated, grew wider, multiplied and propagated by means of gradually consuming the DRX regions with the increase of local strains. Those micro shear bands are considered to contribute to synergetic plastic deformation in addition to dislocation slipping at lower strains, while some macro shear bands are regarded as the precursor of fracture at higher strains. Based on the observation results a new DRX mechanism of shear band was proposed. The experimental results in the present work can provide new evidences and novel insights of the shear-band formation, plastic deformation as well as failure mode in UFG alloys under quasi-static loading conditions.

Enhanced corrosion behavior of ultrafine-grained pure titanium in simulated high-temperature seawater

Corrosion behavior of ultrafine-grained (UFG) pure titanium was studied in simulated seawater at high temperature to increase the probability for marine devices. The UFG Ti was prepared by equal channel angular pressing. The grain size was around 450 nm. The results showed that the corrosion current density of UFG Ti was lower than coarse-grained (CG) Ti in 3.5%NaCl solution at 80 °C, and the UFG Ti could resist pitting corrosion preferably. The basal texture of UFG Ti was stronger and the content fraction of TiO2 in the passive film was higher than CG Ti. The enhanced corrosion performance of UFG Ti at high temperature was attributed to the comprehensive impact of grain size, texture and passive film.

Enhanced Erosion Resistance of an Ultrafine-Grained Ti Alloy with a PVD Coating

This paper presents the results of a comprehensive study of the erosive wear resistance, strength, and adhesive characteristics of the high-temperature structural titanium alloy Ti-5.7Al-3.8Mo-1.2Zr-1.3Sn (the Russian grade VT8M-1) with coarse-grained and ultrafine-grained (UFG) structures and a protective erosion-resistant TiVN coating produced by physical vapor deposition (PVD), deposited on the alloy surface. A microscopic analysis of the areas subjected to the action of abrasive particles was performed, and different characters of erosive wear were revealed depending on the structural state of the alloy. The obtained results convincingly demonstrate that by means of refining the grain structure of alloys and depositing a protective ion-plasma TiVN coating on the alloy surface, it is possible to significantly increase the erosion resistance of materials operating under high loads and in aggressive environments.

Adiabatic Shear Failure of Ultrafine Grained Titanium Under Impact Loading: An in-situ Experimental Study

Background: Ultrafine-grained (UFG) titanium, which is with high yield strength, biocompatibility and corrosion resistance, is widely used in biomedical and industrial applications. However, adiabatic shear localization (ASL) is often observed in UFG materials due to their worse deformation stability under impact loading. This instability will easily result in formation of adiabatic shear bands (ASB), a narrow band located in the ASL zoom, and finally cause the fracture of material. The main objective of this work is to study the adiabatic shear behavior of UFG titanium under impact loading, including macro- and micro-properties, temperature rise, ASB failure, etc. Methods: A synchronization apparatus, which consisted of Kolsky bar system, high-speed camera system and high-speed infrared temperature measuring system, was set up to carry out the in-situ study of the mechanical properties, temperature rise, and adiabatic shear failure process of UFG pure titanium. Microstructure of the material was also analyzed in this work. Results: The critical strain of UFG pure titanium for adiabatic shear localization is about 0.37 and 0.69 for UFG Ti and CG Ti, respectively. The peak shear stress of UFG Ti is 500MPa. The propagation velocity of ASB in UFG titanium is 533~800m/s, and 160~320m/s for CG Ti. The temperature rsie within ASB of UFG titanium is 307~732℃, and 212-556℃ for CG Ti. The intense temperature rise is after the peak stress and the initiation of ASB most of the time. Conclusion: UFG Ti has good mechanical properties, however, it is easier to form ASB and cause adiabatic shear failure under impact loading when compared with CG Ti. Temperature rise may not play a major role in the formation of ASB in UFG Ti, but may be the consequence of ASB. Results of this work will help researchers better understand the failure of UFG metals under impact loading.

Fatigue Properties of Ti Alloys with an Ultrafine Grained Structure: Challenges and Achievements

Ultrafine-grained (UFG) structure formation in Ti alloys, by severe plastic deformation (SPD) processing and enhancement of their mechanical properties, including fatigue properties, has been demonstrated in numerous studies in the past 20 years. The present overview analyzes the fatigue properties achieved to date in Ti alloys subjected to SPD. Such aspects are examined as the effect of a UFG structure on the fatigue behavior of commercially pure (CP) Ti, two-phase Ti alloys, using the popular Ti-6Al-4V alloy as an example, as well as on the kinetics and mechanisms of fatigue failure. The prospects and problems of the practical application of UFG Ti materials in medicine and aircraft engine construction are discussed.

A strong and ductile pure titanium

The low strength of pure Ti significantly limits its biomedical applications, although its biocompatibility is the best. Here, by controlled annealing and cryogenic drawing after rolling, we synthesize a set of pure Ti combining the strength of ultrafine-grained Ti and the ductility of coarse-grained Ti. The microstructure is characterized with fine grains (a few microns), abundant twins, and high dislocation density, which enable both short dislocation-slip path for strengthening and enough defects accumulation room for work hardening. Twins provide strengthening due to the subdivision effect of twin lamella on grains and dislocations accumulation near the twin boundaries. High flow stress helps to activate FCC phase transformation at large-strain stage. The excellent ductility is originated from the sustained work hardening enabled by the initial texture, fine grains, the interaction among dislocations, FCC lamellae, and twins.

Fracture of severely plastically deformed titanium

The mechanical properties with emphasis on the fracture behaviour of ultrafine-grained Ti processed by high pressure torsion were evaluated. Through this process a substantial refinement of the microstructure was induced. As a consequence, a pronounced increase of tensile strength was achieved compared to conventional Ti while the ductility exhibited only a minor reduction after processing. The fracture toughness in terms of the critical stress intensity factor and crack tip opening displacement was evaluated in different crack growth directions and showed a pronounced orientation dependency, which can be related to the typically elongated microstructure induced by this deformation method.

Fatigue properties of UFG Ti grade 2 dental implant vs. conventionally tested smooth specimens

Complicated geometry in combination with surface treatment strongly deteriorates fatigue resistance of metallic dental implants. Mechanical properties of pure Ti grade 2, usually used for dental implant production, were shown to be significantly improved due to intensive grain refinement via Conform SPD. The increase of the tensile strength properties was accompanied by a significant increase in the fatigue resistance and fatigue endurance limit. However, the SLA treatment usually used for the implants' surface roughening, resulted in the fatigue properties and endurance limit decrease, while this effect was more pronounced for the ultrafine-grained comparing to the coarse-grained material when tested under tensile-tensile loading mode.The testing of the implants is usually provided under the bending mode. Even though different testing condition for the conventional specimens tests and implants testing was adopted, a numerical study revealed their comparable fatigue properties. The fatigue limit determined for the implants was 105% higher than the one for coarse-grained and only by 4 % lower than the one for ultrafine-grained Ti grade 2.Based on the obtained results, conventional specimens testing can be used for the prediction of the fatigue limit of the implants.