Search Results (24)

In this paper, the impact of mechanical alloying (MA) and spark plasma sintering (SPS) on the phase evolution and mechanical properties development of CoCrFeNiTi high–entropy alloys (HEAs) was investigated. The microstructure and properties of the material were examined, using X-ray diffraction (XRD) for phase identification, scanning electron microscopy (SEM) for surface morphology observation, transmission electron microscopy (TEM) for microstructural analysis, and hardness testing to evaluate mechanical performance. The milled powder exhibited nanocrystalline solid solution microstructure with grain sizes below 48 nm, composed of 83% face–centered cubic (FCC) and 17% body–centered cubic (BCC) phases. Mechanically, the bulk CoCrFeNiTi alloy exhibited exceptional strength attributes, as evidenced by a Vickers hardness value reaching 675 Hv, along with a compressive strength of 1894 MPa and a yield stress of 1238 MPa. These findings suggested that the synergistic effects of mechanical alloying and SPS processing can precisely control the phase stability, microstructure refinement, and property optimization in CoCrFeNiTi HEA, with particular promise for advanced structural applications. Full article

Three alloys differing in their nominal chemical composition (Ni₅₀Ti₅₀, Ni₅₁Ti₄₉, and Ni₅₂Ti₄₈) were produced in the form of powders using high-energy ball milling. Their microstructure, morphology, structure, and phase composition were studied using the X-ray diffraction technique, scanning, and transmission electron microscopy. For the detailed structural analysis, the Rietveld method was used. The results show that each of the alloys consists of three fractions: fine, medium, and thick. The fractions varied in particle/agglomerate size from 200 nm to 800 μm. Additionally, they varied in phase composition. The fine fraction comprised a mixture of amorphous and nanocrystalline phases. Additionally, the medium and coarse phases showed crystalline solid solutions formed on the bases of nickel or titanium, as well as a crystalline bcc phase—a precursor of the parent phase (B2). The largest contribution in the alloy powders, over 80%, comes from the amorphous–nanocrystalline mixture (ANM). The increase in the nickel content resulted in an increase in ANM quantity of 3 wt.%. Similarly, the weight content of the titanium-based solid solution increased to about 7 wt.%. In contrast, the quantity of the nickel-based solid solution decreased from 3 wt.% to approximately 1 wt.% in the Ni₅₀Ti₅₀ and Ni₅₂Ti₄₈ alloys. Full article

Nickel–titanium (NiTi) shape memory alloys are promising materials for orthopedic implants due to their unique mechanical properties, including superelasticity and shape memory effect. However, the high nickel content in NiTi alloys raises concerns about biocompatibility and potential cytotoxic effects. This review focuses on the recent advancements in surface modification techniques aimed at enhancing the properties of NiTi alloys for biomedical applications, with particular emphasis on low-temperature glow discharge plasma oxidation methods. The review explores various surface engineering strategies, including oxidation, nitriding, ion implantation, laser treatments, and the deposition of protective coatings. Among these, low-temperature plasma oxidation stands out for its ability to produce uniform, nanocrystalline layers of titanium dioxide (TiO₂), titanium nitride (TiN), and nitrogen-doped TiO₂ layers, significantly enhancing corrosion resistance, reducing nickel ion release, and promoting osseointegration. Plasma-assisted oxynitriding processes enable the creation of multifunctional coatings with improved mechanical and biological properties. The applications of modified NiTi alloys in orthopedic implants, including spinal fixation devices, joint prostheses, and fracture fixation systems, are also discussed. Despite these promising advancements, challenges remain in achieving large-scale reproducibility, controlling process parameters, and reducing production costs. Future research directions include integrating bioactive and antibacterial coatings, enhancing surface structuring for controlled biological responses, and expanding clinical validation. Addressing these challenges can unlock the full potential of surface-modified NiTi alloys in advanced orthopedic applications for safer, longer-lasting, and more effective medical implants. Full article

Fracture toughness is a critical indicator for the application of NiTi alloys in medical fields. We propose to enhance the fracture toughness of NiTi alloys by controlling the spatial grain size (GS) gradient. Utilizing rolling processes and heat treatment technology, three categories of NiTi alloys with distinct spatial GS distributions were fabricated and subsequently examined through multi-field synchronous fracture tests. It is found that the one with a locally ultra-high GS gradient (20 nm−3.4 μm) has significantly enhanced fracture toughness, which is as high as 412% of that of the normally distributed nano-grains with an average GS of 8 nm and 178% of that of the coarse-grains with an average GS of 100 nm. Theoretical analysis reveals that in such a gradient structure, phase transition in the coarse-grained matrix greatly absorbs the surface energy of subcritical and stable propagation. Meanwhile, the locally non-uniform GS distribution leads to deviation and tortuosity of the crack path, increasing the critical fracture stress. Furthermore, the nanocrystalline clusters distributed in the form of network nodes reduce the stress intensity factor due to their higher elastic modulus compared to the coarse-grained matrix. This work provides guidance for developing new gradient nanostructured NiTi alloys with high fracture toughness. Full article

Background: The NiTi alloy, known for its shape memory and superelasticity, is increasingly used in medicine. However, its high nickel content requires enhanced biocompatibility for long-term implants. Low-temperature plasma treatments under glow-discharge conditions can improve surface properties without compromising mechanical integrity. Methods: This study explores the surface modification of a NiTi alloy by oxidizing it in low-temperature plasma. We examine the impact of process temperatures and sample preparation (mechanical grinding and polishing) on the structure of the produced titanium oxide layers. Surface properties, including topography, morphology, chemical composition, and bioactivity, were analyzed using TEM, SEM, EDS, and an optical profilometer. Bioactivity was assessed through the deposition of calcium phosphate in simulated body fluid (SBF). Results: The low-temperature plasma oxidization produced titanium dioxide layers (29–55 nm thick) with a predominantly nanocrystalline rutile structure. Layer thickness increased with extended processing time and higher temperatures (up to 390 °C), though the relationship was not linear. Higher temperatures led to thicker layers with more precipitates and inhomogeneities. The oxidized layers showed increased bioactivity after 14 and 30 days in SBF. Conclusions: Low-temperature plasma oxidation produces bioactive titanium oxide layers on NiTi alloys, with a structure and properties that can be tuned through process parameters. This method could enhance the biocompatibility of NiTi alloys for medical implants. Full article

Sn–Ni alloy matrix coatings co-deposited with TiO₂ nanoparticles (Evonik P25) were produced utilizing direct (DC) and pulse electrodeposition (PC) from a tin–nickel chloride-fluoride electrolyte with a loading of TiO₂ nanoparticles equal to 20 g/L. The structural and morphological characteristics of the resultant composite coatings were correlated with the compositional modifications that occurred within the alloy matrix and expressed via a) TiO₂ co-deposition rate and b) composition of the matrix; this was due to the application of different current types (DC or PC electrodeposition), and different current density values. The results demonstrated that under DC electrodeposition, the current density exhibited a more significant impact on the composition of the alloy matrix than on the incorporation rate of the TiO₂ nanoparticles. Additionally, PC electrodeposition favored the incorporation rate of TiO₂ nanoparticles only when applying a low peak current density (J_p = 1 Adm⁻²). All of the composite coatings exhibited the characteristic cauliflower-like structure, and were characterized as nano-crystalline. The composites’ surface roughness demonstrated a significant influence from the TiO₂ incorporation rate. However, in terms of microhardness, higher co-deposition rates of embedded TiO₂ nanoparticles within the alloy matrix were associated with decreased microhardness values. The best wear performance was achieved for the composite produced utilizing DC electrodeposition at J = 1 Adm⁻², which also demonstrated the best photocatalytic behavior under UV irradiation. The corrosion study of the composite coatings revealed that they exhibit passivation, even at elevated anodic potentials. Full article

The present study elucidates the impact of glow discharge oxidation within a low-temperature plasma environment on the bioactivity characteristics of an NiTi shape memory alloy. The properties of the produced surface layers, such as structure (TEM observations), surface morphology (SEM observations), chemical and phase composition (EDS and XRD measurements), wettability (optical gonimeter), and the biological response of osteoblasts and platelets to the oxidized surface compared with the NiTi alloy without a surface layer are presented. The presented surface modification of the NiTi shape memory alloy, achieved through oxidizing in a low-temperature plasma environment, led to the creation of a continuous surface layer composed of nanocrystalline titanium oxide TiO₂ (rutile). The findings obtained from this study provide evidence that the oxidized layer augments the bioactivity of the shape memory alloy. This augmentation was substantiated through the spontaneous biomimetic deposition of apatite from a simulated body fluid (SBF) solution. Furthermore, the modified surface exhibited improved osteoblast proliferation, and enhanced platelet adhesion and activation. This proposed surface modification strategy holds promise as a prospective solution to enhance the biocompatibility and bioactivity of NiTi shape memory alloy intended for prolonged use in bone implant applications. Full article

High-pressure torsion (HPT) was applied for the Ni_49.6Ti_35.4Hf₁₅ (at.%) alloy up to 1/4, 2 and 16 turns under a pressure of 4.0 GPa. The samples were examined using X-ray diffraction (XRD), transmission electron microscope (TEM) and microhardness measurements. The results indicate that the mixture of an amorphous and nanocrystalline microstructure developed in the investigated NiTiHf alloy as the number of HPT turns was increased to two. The average hardness of the samples increased from 330 Hv to 500 Hv after 16 turns of HPT. Very fine martensite developed when the HPT-processed samples were annealed at 550 °C and the finer microstructures were attained with higher HPT turns. Differential scanning calorimetry (DSC) tests were performed in the post-HPT annealing samples to clarify the transformation behavior after severe plastic deformation in HPT and subsequent annealing, so as to provide an experimental basis for the application of the shape memory alloy. The transformation temperature of the alloy decreased remarkably when the number of turns of HPT reached 16. It is suggested that the deformation extent and annealing temperatures should be considered in order to maintain a high transformation temperature while utilizing the strengthening effect of HPT in the NiTiHf alloy. Full article

In this paper, the fatigue resistance of superelastic NiTi shape memory alloy (SMA) wires was improved by combining mechanical training and nanocrystallization. Fatigue tests were performed after mechanical training with a peak stress of 600 MPa for 60 cycles of nanocrystalline (NC) NiTi wires, and the associated microscopic mechanism was investigated by using transmission electron microscopy (TEM) and transmission Kikuchi diffraction (TKD). The results showed that stress-controlled training effectively improved the functional stability (the accumulated residual strain decreased by 83.8% in the first 5000 cycles) of NC NiTi SMA wires, as well as increased the average structural fatigue life by 187.4% (from 4538 cycles to 13,040 cycles). TEM observations and TKD results revealed that training-induced dislocations resulted in lattice rotation and preferential grain orientation. The finite element method (FEM) simulation results indicated that the training-induced preferential grain orientation tended to decrease the local stress concentration and strain energy density. Combined with fractography analysis, the uniform deformation caused by mechanical training changed the crack growth mode from multi-regional propagation to single-regional propagation, improving the structural fatigue life. Full article

The effect of a promising method of performing a thermomechanical treatment which provides the nanocrystalline structure formation in bulk NiTi shape memory alloy samples and a corresponding improvement to their properties was studied in the present work. The bi-axial severe plastic deformation of Ti-50.7at.%Ni alloy was carried out on the MaxStrain module of the Gleeble system at 350 and 330 °C with accumulated true strains of e = 6.6–9.5. The obtained structure and its mechanical and functional properties and martensitic transformations were studied using DSC, X-ray diffractometry, and TEM. A nanocrystalline structure with a grain/subgrain size of below 80 nm was formed in bulk nickel-enriched NiTi alloy after the MaxStrain deformation at 330 °C with e = 9.5. The application of MaxStrain leads to the formation of a nanocrystalline structure that is characterized by the appearance of a nano-sized grains and subgrains with equiaxed and elongated shapes and a high free dislocation density. After the MaxStrain deformation at 330 °C with e = 9.5 was performed, the completely nanocrystalline structure with the grain/subgrain size of below 80 nm was formed in bulk nickel-enriched NiTi alloy for the first time. The resulting structure provides a total recoverable strain of 12%, which exceeds the highest values that have been reported for bulk nickel-enriched NiTi samples. Full article

This paper presents the results of a transmission electron microscope study of the influence of the size, morphology, and spatial distribution of coherent Ti₃Ni₄ particles on the nature of the R transformation; the morphology of the R phase; and the deformation response depending on the aging temperature in nanocrystalline Ti–50.9 at.% Ni alloy with a grain–subgrain structure. It has been established that with an increase in the aging temperature, the size and spatial distribution of Ti₃Ni₄ particles change from being located on dislocations at an aging temperature of 300 °C to precipitation at sub-boundaries at an aging temperature of 400 °C, 450 °C. Correspondingly, the morphology of the R phase changes from nanodomain-like to a lamellar self-accommodation structure. Studies have shown that the morphology of the R phase, in turn, affects the deformation response of the material. In the case of lamellar self-accommodation morphology, localized R transformation develops in a Lüders-like manner. Full article

The involvement of magnesium matrix composite enhanced by metal particles, the development of low lattice mismatch interface, and the refining of particle size are all of great significance in improving strengthening efficiency. In this work, nano-crystalline Ti/Mg-9Al-Zn-0.3Mn composites were prepared by mechanical milling. The microstructure was characterized and the mechanical property was measured. After mechanical milling, the grain of the Mg matrix was refined to ~72 nm. Ti particles were smashed to submicron scale, and dispersed in the Mg matrix. In total, 68% of Ti particles were nano-scale and the average particle size was 133 nm. A nano-scale Mg₁₇Al₁₂ precipitate was found and the average particle size was approximately 44 nm. Meanwhile, coherent interfaces of Ti/Mg and Mg₁₇Al₁₂/Mg were observed, and it was found that the (101)Mg plane and (100)Ti plane inclined 12° and [044]Mg₁₇Al₁₂ was parallel to [010]Mg. The hardness of the milled Ti/Mg-9Al-Zn-0.3Mn composite was 1.98 GPa, 247% higher than the initial alloy. Milled Mg-9Al-Zn-0.3Mn alloy under the same preparation processing was used as a comparison, and the value of hardness was 1.53 GPa. Tiny Ti particles displayed excellent strengthening efficiency. Strengthening mechanisms of the milled Ti/Mg-9Al-Zn-0.3Mn composite were analyzed and the main strengthening mechanisms included the strengthening of grain boundary strengthening, Orowan strengthening, dislocation strengthening, solid solution strengthening and load-bearing strengthening, which accounted for 56.3%, 18.2%, 17.4%, 4.7% and 3.5%, respectively. Full article

Antibacterial agents derived from conventional organic compounds have traditionally been employed as a biofilm protective coating for many years. These agents, on the other hand, often include toxic components that are potentially hazardous to humans. Multiple approaches have been investigated over the last two decades, including the use of various metallic and oxide materials, in order to produce a diverse variety of usable coating layers. When it comes to material coating approaches, the cold spray technique, which is a solid-state method that works well with nanopowders, has shown superior performance. Its capacity to produce unique material coating in ways that are not possible with other thermal methods is the primary reason for its importance in contemporary production. The present work has been addressed in part to explore the possibility of employing mechanically alloyed Cu₅₀(Ti_50−xNi_x)_x; x = 10, 20, 30, and 40 at.% metallic glass powders, for producing an antibiofilm/SUS304 surface protective coating, using the cold spray approach. In this study, elemental Cu, Ti, and Ni powders were low-energy ball milled for 100 h to fabricate metallic glassy powders with different Ni contents. The as-prepared metallic glassy powders were utilized to coat SUS304 sheets, using the cold spraying process. With high nanohardness values, the as-fabricated coating material, in particular Cu₅₀Ti₂₀Ni_30, demonstrated remarkable performance in comparison to other materials in its class. Furthermore, it displayed excellent wear resistance while maintaining a low coefficient of friction, with values ranging from 0.32 to 0.45 in the tested range. E. coli biofilms were formed on 20 mm² SUS304 sheet coated coupons, which had been injected with 1.5 108 CFU mL⁻¹ of the bacterium. With the use of nanocrystalline Cu-based powders, it is feasible to achieve considerable biofilm inhibition, which is a practical strategy for accomplishing the suppression of biofilm formation. Full article

An electron microscopic study of the evolution of the size, morphology, and spatial distribution of coherent Ti₃Ni₄ particles with a change in the aging temperature in a nanocrystalline (NC) Ti-50.9 at % Ni alloy with an inhomogeneous grain–subgrain B2-austenitic nanostructure has been carried out. It was found that with an increase in the aging temperature, along with a change in the size and shape of Ti₃Ni₄ nanoparticles, their spatial distribution changes from location at dislocations to precipitates at subboundaries. Research has shown that the presence of different types of internal interfaces in the nanostructure contributes to the heterogeneous distribution of coherent Ti₃Ni₄ nanoparticles in the volume of the B2 matrix, which is associated with the precipitation of particles in the region of low-angle subboundaries and the suppression of the Ti₃Ni₄ precipitation in nanograins with high-angle boundaries. The difference in the structural-phase state of nanograins and subgrains regions is the main reason for the implementation of the anomalous R-phase transformation effect in the sequence of multistage martensitic transformations B2↔R↔B19′. Full article

In this article, the microstructure and mechanical behavior of the Ti_49.1Ni_50.9 alloy with a high content of nickel in a coarse-grained state, obtained by quenching, ultrafine-grained (obtained through the equal-channel angular pressing (ECAP) method) and nanocrystalline (high pressure torsion (HPT) + annealing), were investigated using mechanical tensile tests at different temperatures. Mechanical tests at different strain rates for determining the parameter of strain rate sensitivity m were carried out. Analysis of m showed that with an increase in the test temperature, an increase in this parameter was observed for all studied states. In addition, this parameter was higher in the ultrafine-grained state than in the coarse-grained state. The activation deformation volume in the ultrafine-grained state was 2–3 times greater than in the coarse-grained state at similar tensile temperatures. Fractographic analysis of samples after mechanical tests was carried out. An increase in the test temperature led to a change in the nature of fracture from quasi-brittle–brittle (with small pits) at room temperature to ductile (with clear dimples) at elevated temperatures. Microstructural studies were carried out after the tensile tests at different temperatures, showing that at elevated test temperatures, the matrix was depleted in nickel with the formation of martensite twins. Full article