Comparative analysis of the physical, chemical, and microbiological properties of Ti-6Al-4V disks produced by different methods and subjected to surface treatments.

STATEMENT OF PROBLEM: To improve the osseointegration of dental implants and reduce microbiological growth, different micro- and nanoscale surface topographies can be used. PURPOSE: The purpose of this in vitro study was to evaluate the influence of Ti-6Al-4V with 4 surfaces, machined (DU), machined+hydroxyapatite (DUHAp), machined+acid-alkali treatment (DUAA), and additive manufacturing (DMA), on the physical, chemical, and microbiological properties. MATERIAL AND METHODS: The topography of Ti-6Al-4V disks with the 4 surfaces was evaluated by scanning electron microscopy (SEM), the chemical composition by energy dispersive X-ray spectroscopy (EDS), and the crystalline structure by X-ray diffraction (XRD). Physical and chemical properties were analyzed by using wettability and surface free energy, roughness, and microbial adhesion against Staphylococcus aureus by colony forming units (CFU). One-way ANOVA analysis of variance and the Tukey multiple comparisons test were applied to evaluate the data, except CFU, which was submitted to the Kruskal-Wallis nonparametric test (α=.05). RESULTS: DU photomicrographs showed a topography characteristic of a polished machined surface, DUHAp and DUAA exhibited patterns corresponding to the surface modifications performed, and in DMA the presence of partially fused spherical particles was observed. The EDS identified chemical elements inherent in the Ti-6Al-4V, and the DUHAp and DUAA disks also had the ions from the treatments applied. XRD patterns revealed similarities between DU and DMA, as well as characteristic peaks of hydroxyapatite (HA) in the DUHAp disk and the DUAA. Compared with DU and DMA the DUHAp and DUAA groups showed hydrophilic behavior with smaller contact angles and higher surface free energy (P<.05). DMA showed a higher mean value of roughness, different from the others (P<.05), and a higher CFU for S. aureus (P=.006). CONCLUSIONS: DUHAp and DUAA showed similar behaviors regarding wettability, surface free energy, and bacterial adhesion. Among the untreated groups, DMA exhibited higher roughness, bacterial adhesion, and lower wettability and surface free energy.

Analysis of stress/strain distribution in dental mini-implants manufactured by additive manufacturing and machining.

The study aimed to analyze the stress/strain distribution of new designs of mini-implants manufactured by machining and additive manufacturing. Four designs were evaluated (Ø2.0 mm × 10 mm): Intra-lock, helical, threaded machined (MN threaded) and threaded by additive manufacturing (AM threaded). Analysis of stress was performed through photoelastic analysis (100 N axial/oblique loads) and analysis of strain by digital image correlation (DIC) (250 N axial/100 N oblique load). Data distribution was verified using the Shapiro-Wilk test and a significance level of 5% was adopted. Quantitative data were analyzed using the non-parametric Kruskal-Wallis test. In photoelastic analysis, the Intra-lock mini-implant showed the highest stresses in the cervical (104 kPa), middle (108 kPa), and apical (212 kPa) thirds. Higher stresses were observed in the oblique loading situation for all designs. For DIC analysis, axial loading, a significant difference was observed for the AM Threaded mini-implants about the other designs in the cervical third (p = .04), with the highest strain value 47 µÎµ [10; 76]. In oblique loading, a significant difference between the mini-implants was observed in the middle and apical thirds, with higher strains for the AM threaded design -185 µÎµ [-173; 162] (p = .009) and 242 µÎµ [87; 372] (p = .013), respectively. In general, the influence of different mini-implant designs and the additive manufacturing method on the stress/strain was observed, in the photoelastic and DIC analysis. The evaluated designs demonstrated a lower concentration of stress/strain in the cervical region compared to the apical region, and higher stress/strain in situations of oblique load compared with axial load.

Comparison of hydrophilic and hydrophobic nano topographic surfaces of titanium alloys on pre-osteoblastic cell interaction.

This work aimed to assess the influence of different structured substrates with hydrophilic and hydrophobic properties on micro and nano topographies developed on titanium alloys over pre-osteoblastic cell behavior. Nano topography influences small dimension levels of cell morphology by inducing filopodia formation in cell membranes, irrespectively to the wettability behavior of the surface. Therefore, micro and nanostructured surfaces of titanium-based samples using different techniques of surface modification processing, such as chemical treatments, micro-arc anodic oxidation (MAO), and MAO combined to laser irradiation were developed. Isotropic and anisotropic texture morphologies, wettability, topological parameters and compositional alterations were measured after the surface treatments. Finally, cell viability, adhesion and morphological responses were assessed to investigate the influence of distinct topologies on osteoblastic cells aiming to encounter the conditions to better promote mineralization events. Our study demonstrated that the hydrophilic behavior improves cell adhesion, amplified when effective surface area increases. Surfaces presenting nano topography have a direct influence on cell morphology and play a key role for filopodia formation.

Dental mini-implant designs to support overdentures: Development, biomechanical evaluation, and 3D digital image correlation.

STATEMENT OF PROBLEM: Custom mini-implants are needed for edentulous patients with extensive mandibular deficiencies where endosteal placement is not possible. However, the best design for these mini-implants is unclear. PURPOSE: The purpose of this in vitro study was to develop 2 dental mini-implant designs to support mandibular overdentures and evaluate the effect of their geometries on primary stability and stress distribution. MATERIAL AND METHODS: Two mini-implant designs were developed with changes in the shape, size, and arrangement of threads and chamfers. The experimental mini-implants were made of Grade V titanium alloy (Ti-6Al-4V), (Ø2.0×10 mm) and submitted to a nanoscale surface treatment. Thirty mini-implants (n=10) were placed into fresh swine bones: experimental-threaded, experimental-helical, and a commercially available product model (Intra-Lock System) as the control. The biomechanical evaluations of the experimental mini-implants were compared with those of the control in terms of primary stability, through insertion torque (IT), and with the pullout test. The analysis of stress distribution was performed by using the method of 3D digital image correlation under 250-N axial load and 100-N oblique (30-degree angled model) load. The data were analyzed by ANOVA and the Tukey HSD test (α=.05). RESULTS: The IT and pullout test presented a statistically significant difference for all mini-implants (P<.05), with higher IT for the experimental-threaded and maximum pullout force for the control, followed by threaded (P=.001) and helical (P=.001). Regarding the 3D digital image correlation, a lower incidence of stress was found in the cervical third for all mini-implants. No statistically significant differences were found between the designs evaluated (P>.05). CONCLUSIONS: Comparing the experimental mini-implants with the commercially available control, the experimental-threaded model presented greater primary stability, and all mini-implants showed less stress in the cervical third.

Analysis of the mechanical and physicochemical properties of Ti-6Al-4 V discs obtained by selective laser melting and subtractive manufacturing method.

The surface properties of titanium and its alloys are commonly modified by different techniques, including additive manufacturing (AM), to improve the osseointegration of dental implants. The aim of this study was to evaluate and compare the wettability, topography, chemistry, and structure of titanium-aluminum-vanadium (Ti-6Al-4 V) discs fabricated by selective laser melting (SLM) and subtractive manufacturing (conventional machining). Three different groups were evaluated: selective laser melting (SLM); conventional machining with H3 PO4 + NaOH surface treatment (CM + ST); and conventional machining without surface treatment (CM), including analysis of wettability and roughness, morphological and chemical analyses by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX), and structural characterization analysis by computed tomography (micro-CT), and X-ray diffraction (XRD). The results showed that SLM surface had higher roughness (9.09 ± 1.94 Ra; 51.93 ± 11.59 Rz; 11.03 ± 1.95 Sa) and lower wettability (103.23° ± 13) than CM (0.06 ± 0.01 Ra; 0.42 ± 0.078 Rz; 0.07 ± 0.01 Sa) (76.95° ± 4.18) and CM + ST (0.17 ± 0.38 Ra; 0.88 ± 0.15 Rz; 0.18 ± 0.04 Sa) (18.55° ± 6.47) (p < 0.05). SEM images also proved the higher roughness of SLM surface, and CM + ST discs showed a topography resembling a sponge, characteristic of the nanometric treatment applied. EDX and XRD found no differences between the different surfaces, and micro-CT demonstrated the solid characteristic of the SLM disc. Compared with conventional machining, the SLM technique resulted in higher roughness and lower wettability. Meanwhile, the chemical properties and structure of the titanium alloy was not altered by the technique.

Comparative analysis of corrosion resistance between beta titanium and Ti-6Al-4V alloys: A systematic review.

BACKGROUND: The knowledge of the electrochemical property (corrosion resistance) of beta titanium alloys compared to Ti-6Al-4 V for implants is relevant because of the potential cytotoxic effects that the released ions could cause to long-term health. OBJECTIVES: The objective of this systematic review was to seek information on the electrochemical properties (corrosion resistance) of beta titanium alloys compared to Ti-6Al-4 V since the awareness of the electrochemical behavior of the implant surface in the medium is essential for the best indication of the alloys or compositional changes, which may promote benefits to bone-implant interaction in all areas that this procedure is required. METHODS: The PubMed, LILACS, COCHRANE Library, and Science Direct databases were electronically searched for the terms: dental implants AND beta-titanium AND Ti-6Al-4 V AND electrochemical technics. The inclusion criteria were research articles that studied beta-titanium compared to Ti-6Al-4 V using electrochemical techniques in electrolytes of chemical composition similar to body fluid, published in English, between 2000 and 2020. Articles that did not compare the corrosion resistance of these alloys in electrolytes similar to body fluids were excluded. RESULTS: A total of 189 articles were restored and selected by title and/or abstract according to the inclusion and exclusion criteria, which resulted in 15 articles that were reduced to 8 after read in full. The studies in vitro evaluated the corrosion resistance in electrolytes Hank, Ringer, SBF, and 0.9 % NaCl, between beta titanium alloys, obtained by arc fusion or bars stock, and Ti-6Al-4 V, for dental or biomedical implants submitted to surface treatments by heat treatment, plasma electrolytic oxidation (PEO), alkaline treatment, and thermomechanical. CONCLUSION: The evaluated literature allowed to determine that 1) The oxides Nb2O 5, Ta2O 5, and ZrO2 have higher stability and protection quality than that of TiO2 modified by the oxides of Al and V; 2) A higher modulus of elasticity of the Ti-6Al-4 V alloy favors protection against corrosion by maintaining a thicker and more firmly adhered oxide layer; 3) The increase in the thickness of the Ti alloys superficial layer contributes to the improvement of the corrosion resistance.

Formation and stability of complex metallic phases including quasicrystals explored through combinatorial methods.

Aluminum-based quasicrystals typically form across narrow composition ranges within binary to quaternary alloys, which makes their fabrication and characterization challenging. Here, we use combinatorial approaches together with fast characterization techniques to study a wide compositional range including known quasicrystal forming compositions. Specifically, we use magnetron co-sputtering to fabricate libraries of ~140 Al-Cu-Fe and ~300 Al-Cu-Fe-Cr alloys. The alloys compositions are measured through automated energy dispersive X-ray spectroscopy. Phase formation and thermal stability are investigated for different thermal processing conditions (as-sputtered and annealed at 400 °C, 520 °C and 600 °C for Al-Cu-Fe libraries; annealed at 600 °C for Al-Cu-Fe-Cr libraries) using automated X-ray diffraction and transmission electron microscopy. In both systems the compositional regions across which the quasicrystalline phase forms are identified. In particular, we demonstrate that the quasicrystalline phase forms across an unusually broad composition range in the Al-Cu-Fe-Cr system. Additionally, some of the considered alloys vitrify during sputtering, which also allows us to study their nucleation behavior. We find that phases with polytetrahedral symmetry, such as the icosahedral quasicrystal and the λ-Al13Fe4 phase, exhibit higher nucleation rates but lower growth rates, as compared to other phases with a lower degree of polytetrahedral order. Altogether, the here used combinatorial approach is powerful to identify compositional regions of quasicrystals.

Fatigue resistance, electrochemical corrosion and biological response of Ti-15Mo with surface modified by amorphous TiO2 nanotubes layer.

The objective of this work was a systemic evaluation of the anodizing treatment in a ß-type Ti-15Mo alloy to grow a TiO2 nanostructured layer for osseointegration improvement. The technical viability of the surface modification was assessed based on the resistance to mechanical fatigue, electrochemical corrosion, and biological response. By using an organic solution of NH4 F in ethylene glycol, a well-organized array of 90 nm diameter nanotubes was obtained with a potential of 40 V for 6 h, while undefined nanotubes of 25 nm diameter were formed with a potential of 20 V for 1 h. Nevertheless, the production of the 90 nm diameter nanotubes was followed by micrometer pits that significantly reduced the fatigue performance. The undefined nanotubes of 25 nm diameter, besides the greater cell viability and improved osteoblastic cell differentiation in comparison to the as-polished surface, were not deleterious to the fatigue and corrosion properties. This result strengthens the necessity of an overall evaluation of the anodizing treatment, particularly the fatigue resistance, before suggesting it for the design of implants. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 107B: 86-96, 2019.

Characterization and Corrosion Resistance of Boron-Containing-Austenitic Stainless Steels Produced by Rapid Solidification Techniques.

The composition of a commercial duplex stainless steel was modified with boron additions (3.5, 4.5, and 5.5 wt.%) and processed by rapid-quenching techniques: Melt-spinning, copper-mold casting, and high-velocity oxygen fuel (HVOF). Spray deposition was also used to produce alloys as the process may induce rapid-solidified-like microstructures. These processing routes led to microstructures with distinguished corrosion resistance. Among the alloys with different boron contents, the 63.5Fe25Cr7Ni4.5B composition enabled the production of fully amorphous ribbons by melt-spinning. The cooling rate experienced during copper-mold casting, high-velocity oxygen fuel, and spray deposition did not ensure complete amorphization. The crystalline phases thereby formed were (Fe,Cr)2B and (Fe,Mo)3B2 borides in an austenitic-matrix with morphology and refinement dependent of the cooling rates. Fully amorphous 63.5Fe25Cr7Ni4.5B ribbons exhibited outstanding corrosion resistance in chloride-rich alkaline and acid media with negligible corrosion current densities of about 10-8 A/cm² and a broad passivation plateau. Although the specimens of the same composition produced by HVOF process and spray deposition exhibited lower corrosion resistance because of intrinsic porosity and crystalline phases, their corrosion behaviors were superior to those of AISI 1045 steel used as substrate with the advantage to be reinforced with hard borides known to be resistant against wear.

Effect of an amorphous titania nanotubes coating on the fatigue and corrosion behaviors of the biomedical Ti-6Al-4V and Ti-6Al-7Nb alloys.

An array of self-organized TiO2 nanotubes with an amorphous structure was produced on the biomedical Ti-6Al-4V and Ti-6Al-7Nb alloys, and the resulting fatigue and corrosion behaviors were studied. The electrochemical response of the nanotubular oxide surfaces was investigated in Ringer physiological solution through potentiodynamic polarization and electrochemical impedance spectroscopy measurements. The absence of transpassivation in the chloride-containing solution, in addition to the micron-scale values of the passivation current density, indicated the excellent corrosion behavior of the coating and the satisfactory protection against the creation of potential stress concentrators in the surface. Axial fatigue tests were performed in physiological solution on polished and coated conditions, with characterization of the treated surfaces by scanning electron microscopy before and after the tests. The surface modification was not deleterious to the fatigue response of both alloys mainly due to the nano-scale dimension of the nanotubes layer. An estimation based on fracture mechanics revealed that a circumferential crack in the range of 5µm depth would be necessary to affect the fatigue performance, which is far from the thickness of the studied coating, although no cracks were actually observed in the oxide surfaces after the tests.

Fatigue behavior of Ti-6Al-4V alloy in saline solution with the surface modified at a micro- and nanoscale by chemical treatment.

This work evaluated the influence of the surface modification using acid etching combined with alkaline treatment on the fatigue strength of Ti-6Al-4V ELI alloy. The topography developed by chemical surface treatments (CST) was examined by scanning electron microscopy (SEM) and confocal laser scanning microscopy (CLSM). Increased roughness and effective surface area were investigated and compared with the Ti-6Al-4V samples without modification. Surface composition was analyzed by energy dispersive X-ray spectroscopy (EDS). Axial fatigue resistance of polished and modified surfaces was determined by stepwise load increase tests and staircase test method. Light microscopy and SEM were employed to examine the fracture surface of the tested specimens. According to the results, a similar fatigue behavior was found and a negligible difference in the fatigue crack nucleation was observed for the Ti-6Al-4V with CST in comparison to the samples without treatment.

Growth of aluminum-free porous oxide layers on titanium and its alloys Ti-6Al-4V and Ti-6Al-7Nb by micro-arc oxidation.

The growth of oxides on the surfaces of pure Ti and two of its ternary alloys, Ti-6Al-4V and Ti-6Al-7Nb, by micro-arc oxidation (MAO) in a pH 5 phosphate buffer was investigated. The primary aim was to form thick, porous, and aluminum-free oxide layers, because these characteristics favor bonding between bone and metal when the latter is implanted in the human body. On Ti, Ti-6Al-4 V, and Ti-6Al-7Nb, the oxides exhibited breakdown potentials of about 200 V, 130 V, and 140 V, respectively, indicating that the oxide formed on the pure metal is the most stable. The use of the MAO procedure led to the formation of highly porous oxides, with a uniform distribution of pores; the pores varied in size, depending on the anodizing applied voltage and time. Irrespective of the material being anodized, Raman analyses allowed us to determine that the oxide films consisted mainly of the anatase phase of TiO2, and XPS results indicated that this oxide is free of Al and any other alloying element.

Out-of-plane magnetic patterning based on indentation-induced nanocrystallization of a metallic glass.

Periodic arrays of micrometer-sized ferromagnetic structures with perpendicular magnetic anisotropy are prepared by nanoindentation at the surface of a Fe(67.7)B(20)Cr(12)Nb(0.3) glassy ribbon initially showing in-plane magnetic anisotropy. The indented regions exhibit enhanced coercivity and saturation magnetization with respect to the surrounding nondeformed matrix. These effects are due to a mechanically driven selective nanocrystallization of the metallic glass, induced by nanoindentation, even without the need for thermal annealing. In addition, while the amorphous matrix becomes paramagnetic above 325 K, the crystallized regions (consisting of alpha-Fe) remain ferromagnetic upon heating to high temperatures. The local change in the magnetic anisotropy direction is ascribed to a certain degree of crystallographic texture, together with the inverse magnetostriction effect caused by the compressive indentation stresses.