Titanium Grade 4 (Ti G4) is the most commonly used material for dental implants due to its excellent mechanical properties, chemical stability and biocompatibility. A thin, self-passive oxide layer with protective properties to corrosion is formed on its surface. However, the spontaneous TiO2 layer is chemically unstable. In this work, the impact of autoclaving time on corrosion resistance of Ti G4 in artificial saliva solution with pH = 7.4 at 37 °C was studied. Ti G4 was sandblasted with white Al2O3 particles and autoclaved for 30–120 min. SEM, EDS, 2D roughness profiles, confocal laser scanning microscopy, and a Kelvin scanning probe were used for the surface characterization of the Ti G4 under study. In vitro corrosion resistance tests were conducted using open circuit potential, polarization curves, and electrochemical impedance spectroscopy measurements. It was found that Sa parameter, electron work function, and thickness of the oxide layers, determined based on impedance measurements, increased after autoclaving. The capacitive behavior and high corrosion resistance of tested materials were revealed. The improvement in the corrosion resistance after autoclaving was due to the presence of oxide layers with high chemical stability. The optimal Ti G4 surface for dentistry can be obtained by sandblasting with Al2O3 with an average grain size of 53 µm, followed by autoclaving for 90 min.
This work concerns the development of a method of functionalization of the surface of the biomedical Ti–6Al–7Nb alloy by producing oxide nanotubes (ONTs) with drug-eluting properties. Shaping of the morphology, microstructure, and thickness of the oxide layer was carried out by anodization in an aqueous solution of 1 M ethylene glycol with the addition of 0.2 M NH4F in the voltage range 5–100 V for 15–60 min at room temperature. The characterization of the physicochemical properties of the obtained ONTs was performed using SEM, XPS, and EDAX methods. ONTs have been shown to be composed mainly of TiO2, Al2O3, and Nb2O5. Single-walled ONTs with the largest specific surface area of 600 cm2 cm−2 can be obtained by anodization at 50 V for 60 min. The mechanism of ONT formation on the Ti–6Al–7Nb alloy was studied in detail. Gentamicin sulfate loaded into ONTs was studied using FTIR, TG, DTA, and DTG methods. Drug release kinetics was determined by UV–Vis spectrophotometry. The obtained ONTs can be proposed for use in modern implantology as carriers for drugs delivered locally in inflammatory conditions.
Titanium Grade 4 (Ti G4) is widely used in medicine for dental implants. The failure-free life of implants depends on their properties such as resistance to wear and friction processes. This paper presents an analysis of the influence of sandblasting on tribological wear of commercial dental implants made of TiG4 in artificial saliva. Tribological wear measurements were performed in a reciprocating motion in the ball-on-disc system. The scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM/EDS) method was used to characterize the surface of the implants before and after the tribological wear test. The microhardness of Ti G4 was measured before and after sandblasting by the Vickers method. The contact angle was determined by the method of sitting drop in air. The residual stress test using the X-Ray Diffraction (XRD) single-{hkl} sin2ψ method was carried out. The compressive residual stress of 324(7) MPa and surface hardening of Ti G4 was revealed after sandblasting with Al2O3 particles of 53–75 μm in diameter. It was found that sandblasting changes the surface wettability of Ti G4. The intermediate wettability of the mechanically polished surface and the hydrophobicity of the sandblasted surface was revealed. Sandblasting reduces the tribological wear and friction coefficient of Ti G4 surface in saliva. The three-body abrasion wear mechanism was proposed to explain the tribological wear of Ti G4 in saliva.
Calcium phosphate coatings are able to improve the osseointegration process due to their chemical composition, which is similar to that of bone tissues. In this work, to increase the long-term corrosion resistance and to improve the osseointegration process of commercially pure titanium Grade 4 (CpTi G4), biomimetic amorphous calcium phosphate (ACP) coatings were electrodeposited for the first time from an acetate bath with a pH level of 7.0 and a Ca:P ratio of 1.67. ACP coatings were obtained on CpTi G4 substrate subjected to sandblasting and autoclaving using electrochemically assisted deposition at a potential of −3 V relative to the open circuit potential for 30 min at room temperature. SEM, EDS, 2D roughness profiles, amplitude-sensitive eddy current method, and Kelvin scanning probe were used for the surface characterization of the biomaterial under study. In vitro corrosion resistance tests were conducted for 21 days in artificial saliva using open circuit potential, polarization curves, and electrochemical impedance spectroscopy measurements. The passive-transpassive behavior was revealed for the obtained ACP coatings. The long-term corrosion resistance test showed a deterioration of the protective properties for CpTi G4 uncoated and coated with ACP with immersion time. The mechanism and kinetics of the pitting corrosion on the CpTi G4|TiO2|ACP coating system are discussed in detail.
In the group of vanadium-free titanium alloys used for applications for long-term implants, the Ti-13Zr-13Nb alloy has recently been proposed. The production of a porous layer of oxide nanotubes (ONTs) with a wide range of geometries and lengths on the Ti-13Zr-13Nb alloy surface can increase its osteoinductive properties and enable intelligent drug delivery. This work concerns developing a method of electrochemical modification of the Ti-13Zr-13Nb alloy surface to obtain third-generation ONTs. The effect of the anodizing voltage on the microstructure and thickness of the obtained oxide layers was conducted in 1 M C2H6O2 + 4 wt% NH4F electrolyte in the voltage range 5–35 V for 120 min at room temperature. The obtained third-generation ONTs were characterized using SEM, EDS, SKP, and 2D roughness profiles methods. The preliminary assessment of corrosion resistance carried out in accelerated corrosion tests in the artificial atmosphere showed the high quality of the newly developed ONTs and the slight influence of neutral salt spray on their micromechanical properties.
Titanium and its alloys are among the most promising biomaterials for medical applications. In this work, the isothermal oxidation of Ti-6Al-7Nb biomedical alloy towards improving its mechanical properties, corrosion resistance, and bioactivity has been developed. The oxide layers were formed at 600, 700, and 800 °C for 72 h. Scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), 3D profilometry, and microindentation test, were used to characterize microstructure, surface geometrical structure, and the hardness of the diphase (α + β) Ti-6Al-7Nb alloy after oxidation, respectively. In vitro corrosion resistance tests were carried out in a saline solution at 37 °C using the open-circuit potential method and potentiodynamic measurements. Electronic properties in the air were studied using the Scanning Kelvin Probe (SKP) technique. The bioactivity test was conducted by soaking the alkali- and heat-treated samples in simulated body fluid for 7 days. The presence of apatite was confirmed using SEM/EDS and Fourier Transform Infrared Spectroscopy (FTIR) studies. The thickness of oxide layers formed increased with the temperature growth from 0.25 to 5.48 µm. It was found that with increasing isothermal oxidation temperature, the surface roughness, hardness, corrosion resistance, and contact potential difference increased. The Ti-6Al-7Nb alloy after oxidation revealed the HAp-forming ability in a biological environment.
Three-dimensional printing is a dynamically developing field of industry. Its main advantage is the small amount of waste, no need to use specialized tools, and easy control of the mechanical properties of the printed model. One of the most popular techniques of 3D printing is FDM. The main factor influencing the mechanical properties of 3D-printed materials is the filling density. The aim of this study was to determine the mechanical properties of porous structures with a porosity gradient of PLA samples printed using the FDM technique. The accuracy of mapping the structures by computed tomography was assessed, and then a static compression test was performed. It has been shown that the strength properties increased with the increase in the filling density. The highest value of compression strength, amounting to 41.2 MPa, was observed for samples made of PLA with an 80% filling degree, whereas the lowest value of compression strength was found in PLA-T samples with a filling degree of 10%, reaching only 0.6 MPa. It was found that not only the core filling density, but also the outer layers, influences the mechanical properties. The assessment of spatial architecture allowed for a qualitative and quantitative assessment. The obtained images from the computed tomograph showed that the designed sample models were correctly reproduced in the entire volume.
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