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Institute
BTU
The microstructural and functional behavior of TiNi-based wires with a silver content of 0–1.5 at.% was evaluated. The concentration range for Ag doping determined for the TiNi wires with potential for the medical industry was 0–0.2 at.%. Microstructure analysis of TiNi wires with different silver contents at room temperature indicated a multiphase structural state. Various internal structures with tangled grain boundaries were formed by intense plastic deformation. The nanocrystalline structure and phase state of wire with the minimum silver content (0.1 at.% Ag) provide full shape recovery, the greatest reversible strain, and optimal strength and ductility. TiNi ingots with a high Ag content (0.5–1.5 at.%) cracked under minimum load due to excess silver that crystallized along the grain boundaries and broke cohesion bonds between the TiNi grains.
β-type Ti–20Nb–13Zr alloys with low Young’s modulus were prepared at different sintering temperatures (950, 1050, 1150, and 1250 °C). The morphological and structural characteristics of as-prepared samples were investigated by several methods. Wear tests were conducted using a ball-on-plate type oscillating tribometer under different applied loads (2, 10, and 20 N). The morphological characterization indicated that the mean pore and crystallite size continuously decreased with increasing sintering temperature to reach lowest values of 40 nm and 38 nm at 1250 °C, respectively. The relative density of the 1250 °C sintered sample was as high as 98.7%. Moreover, the higher sintering temperature resulted in higher relative density and closed porosity of the sample. Both the friction coefficient and wear rate were lower in the sample sintered at 1250 °C as compared to other samples. This enhancement in tribological properties was attributed to a closed porosity.
Ti–Ni powder compacts were prepared by mechanical alloying (MA), followed by hot isostatic pressing (HIP). Afterwards, the samples were sintered at different temperatures (950, 1050, 1150 and 1250 °C). Microhardness, density, crystallite size as well as microstrain of the sintered samples were measured and analyzed. Wear characteristics in phosphate-buffered saline (PBS) solution was tested under different applied loads of 2 N, 10 N, and 20 N, respectively. The results indicated that the crystallite size continuously decreases with increasing sintering temperature and reaches the lowest value of 31.3 nm at 1250 °C. The relative density of the sample sintered at 1250 °C is 98.0%. Moreover, the higher sintering temperatures lead to the higher relative density and the increase in hardness and young’s modulus of the sample. At the same time the friction coefficient and wear rate were lower for the samples sintered at 1250 °C. This improvement in friction and wear resistance is attributed to the grain size refinement. Ti–Ni sintered at 1250 °C showed good tribological performance under all test conditions.
The objective of this study was to examine the mechanism how the surface of porous TiNi compounds produced by SHS method evolves. The prepared samples were investigated using light-microscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive x-ray spectroscopy (EDS). The results indicated that the surface of all pores is represented by a granular stratum due to dendrite liquation by peritectic crystallization mechanism. The voids of 2–15 μm in size are formed owing to a capillary spreading of the liquid. Reaction gases with dissociated carbon, nitrogen, and oxygen are responsible for heat-and-mass transfer through the forming pores. High pressure-temperature effect of reaction gases on the melt causes the forming voids to coalesce, as well as transfers the peritectic liquid (PL) throughout the open pores catalyzing a distinctive spitted topography. It is through the chemisorption of gasiform nonmetallics by the pore surface melt, where these impurities are chemically bound, that it was formed a massive corrosion-resistant amorphous-nanocrystalline stratified shell deduced as an intermetallic oxycarbonitride layer.
Structural, and tribological properties of nanostructured α + β type titanium alloys for total hip
(2022)
Titanium alloys are in demand for various biomedical applications and the most popular among them being, Ti–6Al–4V. Hence, in this study, Ti–6Al–7Nb are fabricated through the route of mechanical milling using different sintering temperatures. X-ray diffraction and hardness tests were conducted to characterize the developed sams to evaluate the effect of sintering temperatures on the structural and mechanical properties. It is observed that the sams sintered at a temperature of 1250 °C had the smallest crystallite and pore size, with enhanced relative density and mechanical properties. Tribological tests were conducted at varying normal loads to characterize the wear and frictional behaviour and showed that the sams sintered at 1250 °C presented the lowest friction coefficient and wear rate.
The aim of this study was the comparative analysis of in vitro bio-testing of solid and porous TiNi samples with modified surfaces (intact, oxidated, and etched). Tests for cytocompatibility, hemolysis, and cytotoxicity (MTT) as well as visualization by confocal and scanning electron microscopy have shown that the chemically modified samples are the most cytocompatible. The intact and etched samples did not induce hemolysis greater than 2%, and thus they comply with the ISO 10993-4:2018 standard for hemolysis by blood-contacting biomaterials. Direct culture of etched samples with MCF-7 cells and human leukocytes showed low cytotoxicity. At the same time, the cytotoxicity of samples oxidated at 500 °C was significantly greater than that of the etched samples. Confocal and electron microscopy also confirmed the abovementioned quantitative data. The cells attached to the etched surface in numbers sufficient for them to be able to grow and proliferate on this substrate in vitro. These findings indicate that solid and porous TiNi alloy with surface modifications achieved by a cost-effective method is biotolerable and promising for clinical use and for tissue engineering.
Comparative study on the high-temperature oxidation resistance of porous and solid TiNi-based alloys
(2021)
The present work aims to characterize the surface features of solid and porous (sintered and SHS) TiNi-based alloys subjected to oxidation at 1000 °C in static air in the context of their resistance to high-temperature atmospheric attack. Clear differences between the intact and oxidated surfaces indicate the complexity of a chemicothermal diffusion process evolving therein. Microscopic and XRD studies showed that the dominant superficial constituent in all oxidated samples is titanium dioxide in the rutile modification. The phase and structural properties of the surface layers suggest that porous sintered and solid alloys are most susceptible to high-temperature corrosion due to bare reactive surfaces, which negatively affects their overall biocompatibility. Surface morphology analysis revealed microporous and loose superficial layers having a thickness of 8–10 and 50–60 μm, respectively in the solid and sintered alloy. Also, these alloys showed a high content of leaching NiO and free Ni within the surface layer. Conversely, a thin (0.5–0.6 μm), dense, and multifarious layer of oxycarbonitrides Ti4Ni2(O,N,C) concealing the porous SHS-TiNi matrix inhibits the negative effect of high-temperature oxidation.
The study aimed to characterize the structural-phase composition of the porous SHS TiNi surface explored by the GIXRD method. The surface layers at a depth of up to 100 nm mainly consist of amorphous nanocrystalline intermetallic oxycarbonitrides Ti₄Ni₂(O,N,C) with nonmetallic inclusions of different structural variants and routes of origin. Fine-porous alloys were synthesized at ignition temperatures of 450-480 °C. A distinct feature of the surface of crystalline phases therein was shown to be a low degree of crystallinity (up to 40%) and presence of multifarious glass and cermet phases evident as NiSi₂, NaAlSiO (SO₄), SiO₂, MgSi₂, and CaCO₃. Conversely, large-pore alloys ignited at temperatures of 280-330 °C have a higher degree of crystallinity (up to 70%). An individually selected GIXRD technique and precision structural phase analysis are capable to determine a set of other superficial nonmetallic and cermet phases reported as CaTiO₃, Si (P2O₇), CaSiO₃, MgAl₂O₄, TiNiAl, as well as the Ti₃SiC₂MAX phase.
In this work, we studied the evolution and features of localized strain fields in porous SHS-TiNi samples. Using the Vic-3D optical system and spayed speckle patterns, a localized plastic flow on the surface of porous plates of 0.85 mm and 2.7 mm thick loaded up to fracture in a quasi-static mode was traced and characterized. As seen, a 0.85 mm thick specimen indicated two strain-hardening distinctive parts in the stress-strain curve. Moreover, regions of localized strain are found that be wider than that of a 2.7 mm thick sample. It can be argued that by combining speckle patterns and quasi-static tension, one can effectively explore and predict the deformation behavior of a designing bone substitute made of porous SHS-TiNi.
Porous TiNi alloys fabricated by self-propagating high-temperature synthesis (SHS) are biomaterials designed for medical application in substituting tissue lesions and they were clinically deployed more than 30 years ago. The SHS process, as a very fast and economically justified route of powder metallurgy, has distinctive features which impart special attributes to the resultant implant, facilitating its integration in terms of bio-mechanical/chemical compatibility. On the phenomenological level, the fact of high biocompatibility of porous SHS TiNi (PTN) material in vivo has been recognized and is not in dispute presently, but the rationale is somewhat disputable. The features of the SHS TiNi process led to a multifarious intermetallic Ti4Ni2(O,N,C)-based constituents in the amorphous-nanocrystalline superficial layer which entirely conceals the matrix and enhances the corrosion resistance of the unwrought alloy. In the current article, we briefly explore issues of the high biocompatibility level on which additional studies could be carried out, as well as recent progress and key fields of clinical application, yet allowing innovative solutions.