Functional Elements Coatings on the Plasma Electrolytic Oxidation-Treated Ti-6Al-4V Alloy by Electrochemical Precipitation Method.

In this study, functional elements coatings on the plasma electrolytic oxidation (PEO)-treated Ti-6Al-4V alloy by electrochemical precipitation method were investigated. Ti-6Al-4V ELI disks were used as specimens for PEO and HA coating. The applied voltage and time were selected to be 280 V and 3 minutes for PEO treatment, respectively. The electrochemical precipitation on the Ti-6Al-4V alloy was carried out using cyclic voltammetry with cycle of 3, 5, 10, and 20 from -1.5 V to 0 V (vs. SCE electrode) in electrolyte containing Ca, P, Mg, Mn, Sr, Zn, and Si ions by cyclic voltammetry after PEO treatment. The morphology changes of the coatings on the PEO treated Ti-6Al-4V alloy surface were observed using FE-SEM and EDS. PEO surface has a uniformly distributed circular shape and a porous surface and the deposition of low cycles in electrolyte containing Mg, Mn, Sr, Zn, and Si-HA coated surfaces show uniform circular and granular structures. The precipitates of Mg, Mn, Sr, Zn, and Si-HA on the PEO treated surface showed a large number of circular particles as the number of deposition cycles increases with a mixture of rod-shaped particles and petal-shaped particles around pores. The precipitate nucleates around the pore and grows rapidly as the cycles increase.

Functional Elements Coatings on Ti-6Al-4V Alloy by Plasma Electrolytic Oxidation for Biomaterials.

In this study, functional elements coatings on Ti-6Al-4V alloy by plasma electrolytic oxidation for biomaterials were studied using various experimental techniques. For this study, Ti-6Al-4V ELI disk (grade 5, Timet Co. Ltd., Japan diameter; 10 mm) were used as the substrate for PEO treatment in the electrolyte containing Ca, P, Si, Zn, and Mn ions. The PEO treatment was performed using a pulsed DC power supply at 280 V for 3 min. The PEO-treated surface was observed with field-emission scanning electron microscope (FE-SEM), and energy dispersive X-ray spectrometry (EDS; Oxford ISIS 310, England), Image Analyzer software, and X-ray diffractometer (TF-XRD, X'pert Philips, Netherlands). The number of pores increases, as the Zn ion content increases. And the number of pores decrease, as the Mn ion content increases. The addition of Zn and Mn ions affects the number and size of pores and the area occupied by the pores. Mn and Zn are distributed around pores and in the pores. Anatase and rutile peaks appear and the HA peak shifted to the left in the case of Mn and Zn ion additions.

Pore Shape Changes and Apatite Formation on Zn and Si Ion-Doped HA Films of Ti-6Al-4V After Plasma Electrolytic Oxidation Treatment.

In this study, pore shape changes and apatite formation on zinc (Zn) and silicon (Si) ion-doped hydroxyapatite (HA) films of Ti-6Al-4V by plasma electrolytic oxidation (PEO) treatment has been investigated by several techniques. The PEO films and the Ti-6Al-4V surface after immersion in SBF were observed by X-ray spectroscopy, field-emission scanning electron microscopy, and energy dispersive X-ray spectroscopy. The number of pores decreased as Zn ion concentration increased from 5Zn to 10Zn. The maximum size of pores were increased from 5Zn to 20Zn concentration, whereas, the minimum size of pores decreased. The amount of bone-like apatite formation for the 5Zn/5Si sample was higher than those of other samples immersed in SBF.

Morphology Changes of Plasma Electrolytic Oxidized Ti-6Al-4V Alloy in the Electrolytes Containing Sr and Si Ions.

In this study, morphology changes of plasma electrolytic oxidized (PEO) Ti-6Al-4V alloy in the electrolytes containing Sr and Si ions were researched using field-emission scanning electron microscope, Image J program thin film X-ray diffraction, and energy dispersive X-ray spectroscopy. Pulsed DC power supplied Ti-6Al-4V alloy was used at a 280 V for 3 minutes in the electrolyte containing Sr and Si ions. To determine cell growth, human embryonic kidney cells 293 were grown at a density of 2 × 105 cells per 1.0 ml in well plates. The pore size decreased, as the content of Sr ion increased, whereas, the number of pores per area increased. The Ca/P ratio of PEO treated in electrolyte containing high Sr concentration showed the higher than those of in electrolyte containing low Sr concentration. The peak of HA is shifted to left side, as the concentration of Sr increased. Also, the number of cells increased, as the concentration of Sr increased.

Hydroxyapatite Coatings Containing Mn and Si on the Oxidized Ti-6Al-4V Alloy for Dental Applications.

The purpose of this study was to investigate hydroxyapatite coatings containing Mn and Si on the oxidized Ti-6Al-4V alloy for dental applications. Dental implant fixture and Ti-6Al-4V ELI disk were used as substrates for plasma electrolytic oxidation (PEO) treatment. PEO treatment was performed at 280 V for 3 min in various solutions. The surface morphologies of the specimens after PEO treatment were observed with a field-emission scanning electron microscope, energy-dispersive X-ray spectroscopy, X-ray diffractometer, and Fourier transform infrared spectroscopy. The breakdown potential for pore formation depended on the added ions in electrolytes. Rough surface with micro-pores was formed after plasma discharge in the electrolytes containing Si and Mn ions. The surface morphologies of implant fixtures were covered with manganese-silicon compounds, as Mn concentration increased. From the XRD analysis, anatase peaks decreased, as Mn and Si contents increased. From the results of FT-IR analysis, Si-HA and Mn-HA was formed on the implant surface.

Electrochemical Deposition of Hydroxyapatite Substituted with Magnesium and Strontium on Ti-6Al-4V Alloy.

In the present study, electrochemical deposition of hydroxyapatite substituted with magnesium and strontium on Ti-6Al-4V alloy have investigated. Mg and Sr-doped HAp was coated using subsequently pulsed electrochemical deposition process at 85 °C in the solution contained Ca, Mg, Sr, and P ion. The morphology of Mg/Sr-HAp formed on implant was investigated using scanning electron microscopy and X-ray diffraction. HAp grain size and XRD intensity decreased with Mg2+ and Sr2+ ions. The initial current density was changed with addition of Mg and Sr ion concentration when the constant voltage was applied to specimens. The morphologies and phase of HAp coated layers were affected by the Mg and Sr ion concentration. Results suggest that Mg/Sr-HAp layer formed on Ti can be a potential candidate for dental materials application.

A Simulated Body Fluid Evaluation of TiO2 Barrier Oxide Layer Formed by Electrochemical Reaction.

The modified surface during implantation is considered to be an effective strategy to improve high adhesion of bone cell and osseointegration activity. In this paper, the TiO2 barrier oxide Layer has been fabricated by using the ion characteristic of an electrolytic solution, the surface characteristics have been investigated by EDS, XPS, and FE-SEM. From the analysis of the chemical states, phosphorus and calcium were observed in the TiO2 barrier layer, which were penetrated from the electrolyte into the oxide layer during deposit process. In addition, Ca 2p spectrum was identified into two peaks for Ca 2p3/2 and 2p1/2 at 347.4 and 351.3 eV, which are related to hydroxyapatite. Also, P spectrum was confirmed into two peaks for P1/2 and P3/2 levels with binding energy 134.2 and 133.4 eV, respectively. Thus, the incorporated phosphate species were found mostly in the forms of HPO-4, PO-3. From the result of biological evaluation in simulated body fluid (SBF), the apatite morphologies were effective for bioactive property on the modified surface.

Surface Characteristics of Nanotube Formed Ti­25Nb­xZr Alloys.

The purpose of this study was to investigate surface characteristics of nanotube formed Ti­25Nb­xZr alloys. Ti­25Nb­xZr ternary alloys with 0­15 wt% Zr were manufactured in a vacuum arcmelting furnace. Ingots of the alloys were homogenized in an Ar atmosphere at 1000 °C for 12 h, followed by quenching in ice water. Nanotube layers were formed by an electrochemical method in 1 M H3PO4 and 0.8 wt% NaF at 30 V for 1 h. As the Zr content of the Ti­25Nb­xZr Alloys increased, the crystals transformed from a needle-like to equiaxed structure. Two nanotube sizes were obtained on the Ti­25Nb­xZr alloys. As the Zr content was increased, the diameters of the larger tubes decreased, whereas those of the smaller tubes increased. However, increased Zr content in the Ti­25Nb­xZr alloys had little effect on wettability.

Effects of Electrolyte Concentration on Formation of Calcium Phosphate Films on Ti­6Al­4V by Electrochemical Deposition.

Nano-sized calcium phosphate film was formed on Ti­6Al­4V alloy using simple electrochemical deposition. Pre-treatment of Ti­6Al­4V alloy was carried out by galvanostatic treatment step which acted as anchorage for growth of the hydroxyapatite during subsequent pulsed electrochemical deposition process at 40 and 85 °C. The phase and morphologies of deposited calcium phosphate were influenced by the electrolyte temperature and electrolyte ratio (Ca/P). The nano needle-like precipitates were formed under 1.67 Ca/P ratio in solution. The needle-like deposits were transferred to the plate-like precipitates in the case of Ca-deficient or Ca-rich electrolyte.

Phenomena of Nano- and Micro-Pore Formation on Ti-(10~50)Ta Alloys by Plasma Electrolytic Oxidation for Dental Implants.

In this study, the phenomena of nano and micro-pore formation on Ti-(10~50)Ta alloys by plasma electrolytic oxidation for dental implants was investigated using various experimental techniques. The Ti­xTa alloys having Ta contents of 10, 30, and 50 wt.% were prepared using arc-melting vacuum furnace. Micro-pore formation was performed using a potentiostat in 1 M H3PO4 electrolyte by using a potentiostat at various applied voltage (180 V, 210 V, and 240 V). The microstructure of Ti­xTa alloys changed from α' phase to ß + α″ phase with Ta content increased. The applied potential increased, the numbers of micro-pore per unit area decreased, whereas the area ratio of occupied by micro-pores increased. The Ta contents increased, the numbers of micro-pore per unit area decreased, whereas the area ratio of occupied by micro-pores increased at 210 V and 240 V. The thickness of oxide layer and micro-pore size can be controlled by applied potential.

Biocompatibility of Mg Ion Doped Hydroxyapatite Films on Ti-6Al-4V Surface by Electrochemical Deposition.

In this study, we prepared magnesium (Mg) doped nano-phase hydroxyapatite (HAp) films on the TiO2 nano-network surface using electrochemical deposition method. Ti-6Al-4V ELI surface was anodized in 5 M NaOH solution at 0.3 A for 10 min. Nano-network TiO2 surface were formed by these anodization steps which acted as templates and anchorage for growth of the Mg doped HAp during subsequent pulsed electrochemical deposition process at 85 degrees C. The phase and morphologies of HAp deposits were influenced by the Mg ion concentration.

Electrochemical Characteristics of Cell Cultured Ti-Nb-Zr Alloys After Nano-Crystallized Si-HA Coating.

The aim of this study was to investigate the electrochemical characteristics of nano crystallized Si-HA coating on Ti-Nb-Zr alloy after human osteoblast like (HOB) cell attachment. The Ti-Nb-Zr alloy was manufactured with 35 wt.% of Nb and 10 wt.% of Zr by arc melting furnace to appropriate physical properties as biomaterials. The HA and Si-substituted coatings were prepared by electron-beam physical vapor deposition method with 0.5, 0.8 and 1.2 wt.% of Si contents, and nano aging treatment was performed 500 degrees C for 1 h. The characteristics of coating surface were analyzed by field emission scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction, respectively. To evaluate of cell attachment on cell cultured surface, the potentiodynamic test was performed on the surface using HOB cells. The results showed that the Si-HA coating surface showed higher tendency of cell attachment than that of single HA coating, corrosion resistance value was increased by dense of cell attachment.

The Control of Nanotube Morphology Using Various Factors for Dental Implant.

The purpose of this study was to investigate the control of nanotube morphology using various factors for dental implant. TiO2 nanotube formation on biomedical grade α+ß type Ti-6Al-4V alloy was investigated using anodization technique as a function of applied DC potential (10 V to 30 V and 30 V to 10 V) and anodization time for 60 min in 1 M H3PO4 with small additions of NaF (0.5 wt.%, and 0.8 wt.%). The microstructure and phase characteristics of surface were examined by optical microscopy, field emission scanning electron microscopy and X-ray diffraction. Also, in order to observe the biocompatibility and surface roughness, wettability and atomic force microscopy of alloy was measured.

Biocompatibility of nanotube formed Ti-30Nb-7Ta alloys.

The purpose of this study was to investigate the biocompatibility of Ti-30Nb-7Ta alloy surface decorated with TiO2 nanotubes by anodization in an electrolyte containing 1 M H3PO4 and 0.8 wt.% NaF with an applied voltage of 10 V for 2 h. The anodization was carried out using a scanning potentiostat. The microstructures of alloys and morphology of the nanotubes were investigated by optical microscopy, field emission scanning electron microscopy, and X-ray diffractometry. In comparison to the Ti-30Nb-3Ta alloy, the Ti-30Nb-7Ta alloy contained a lower amount of α" phase, while the ß phase was higher. In this study, we observed the formation of a spongy porous layer on the Ti-30Nb-7Ta alloy, while the Ti-30Nb and Ti-30Nb-3Ta alloys showed an absence of such a spongy layer.

Nanotube nucleation phenomena on Ti-25Ta-xZr alloys for implants using ATO technique.

The purpose of this study was to investigate nanotube nucleation phenomena on the Ti-25Ta-xZr alloys for implant materials, using an anodic titanium oxide (ATO) technique. Ti-25Ta-(0 wt.%-15 wt.%) Zr alloys were prepared using a vacuum arc-melting furnace. The Ti-25Ta-xZr alloys were then homogenized for 12 hr at 1000 degrees C, followed by water quenching. Formation of the nanotubular oxide surface structure was achieved initially on the Ti-25Ta-xZr alloys by anodization in a 1 M H3PO4 electrolyte containing 0.8 wt.% NaF at room temperature, using a potentiostat. After the first formation of the nanotubes was achieved, this initial nanotube layer was eliminated, and further anodization was carried out repeatedly. The microstructure, phase transformation, and morphology of nanotubular Ti-25Ta-xZr alloys and the process of nanotube growth using this ATO method were analyzed by X-ray diffraction, field-emission scanning electron microscopy, and energy dispersive X-ray spectroscopy. Microstructures of the Ti-25Ta-xZr alloys changed from α" phase to ß phase. Nanotubes formed with the ATO technique had pit-like top holes, with thinner walls and lower contact angle, compared to the initially formed nanotubes.

Surface phenomena of hydroxyapatite film on the nanopore formed Ti-29Nb-xZr alloy by anodization for bioimplants.

In this study, surface phenomena of hydroxyapatite (HA) film on the nanopore formed Ti-29Nb-xZr alloy by anodization for bioimplants have been investigated by electron beam physical vapor deposition (EB-PVD), field emission scanning electron microscope (FE-SEM), X-ray diffractometer (XRD), potentiostat and contact angle. The microstructure of Ti-29Nb-xZr alloys exhibited equiaxed structure and alpha" phase decreased, whereas beta phase increased as Zr content increased. The increment of Zr contents in HA coated nanotubular Ti-29Nb-xZr alloys showed good corrosion potential in 0.9% NaCI solution. The wettability of HA coated nanotubular surface was higher than that of non-coated samples.

Surface observation of nanotube/micropit formed Ti-Nb-xZr alloy for biocompatibility.

To improve bone tissue integration on implant surfaces, nanotube formation and laser texturing techniques have been used to increase the roughness of the implant surfaces. In this study, surface film of nanotube/micropit formed Ti-3ONb-xZr and Ti-30Ta-xZr alloy with low elastic modulus have been investigated using field emission scanning electron microscope (FE-SEM) and energy dispersive X-ray spectroscope (EDS). The alloying elements can play role in controlling the nanotube shape and micropit shape, the highly ordered nanostructure, and contact angle for biocompatibility.

Surface morphology of highly ordered nanotube formed and laser textured beta titanium alloys.

The aim of the present study is to produce and characterize a well-controlled surface texture on Ti-35Nb-xHf alloys to promote osseointegration. Ti-35Nb-xHf (x = 0, 3, 7 and 15 wt.%) alloys were prepared by arc melting and heat treated for 12 hr at 1000 degrees C in an argon atmosphere and then water quenching. For surface texturing, an amplified Ti: sapphire laser system was used for generating 184 femtosecond (FS, 10(-15) sec) laser pulses with the pulse energy over 30 mJ at a 1 kHz repetition rate with a central wavelength of 800 nm. The nanotube formation was achieved by anodizing a Ti-35Nb-xHf alloy in H3PO4 electrolytes containing 0.8 wt.% NaF at room temperature. The surface morphology of nano/micro structure will enhance osseointegration and cell adhesion.

DMP1 and IFITM5 Regulate Osteogenic Differentiation of MC3T3-E1 on PEO-Treated Ti-6Al-4V-Ca2+/Pi surface.

Despite numerous studies on various surface modifications on titanium and its alloys, it remains unclear what kind of titanium-based surface modifications are capable of controlling cell activity. This study aimed to understand the mechanism at the cellular and molecular levels and investigate the in vitro response of osteoblastic MC3T3-E1 cultured on the Ti-6Al-4V surface modified by plasma electrolytic oxidation (PEO) treatment. A Ti-6Al-4V surface was prepared by PEO at 180, 280, and 380 V for 3 or 10 min in an electrolyte containing Ca2+/Pi ions. Our results showed that PEO-treated Ti-6Al-4V-Ca2+/Pi surfaces enhanced the cell attachment and differentiation of MC3T3-E1 compared to the untreated Ti-6Al-4V control but did not affect cytotoxicity as shown by cell proliferation and cell death. Interestingly, on the Ti-6Al-4V-Ca2+/Pi surface treated by PEO at 280 V for 3 or 10 min, MC3T3-E1 showed a higher initial adhesion and mineralization. In addition, the alkaline phosphatase (ALP) activity significantly increased in MC3T3-E1 on the PEO-treated Ti-6Al-4V-Ca2+/Pi (280 V for 3 or 10 min). In RNA-seq analysis, the expression of dentin matrix protein 1 (DMP1), sortilin 1 (Sort1), signal-induced proliferation-associated 1 like 2 (SIPA1L2), and interferon-induced transmembrane protein 5 (IFITM5) was induced during the osteogenic differentiation of MC3T3-E1 on the PEO-treated Ti-6Al-4V-Ca2+/Pi. DMP1 and IFITM5 silencing decreased the expression of bone differentiation-related mRNAs and proteins and ALP activity in MC3T3-E1. These results suggest that the PEO-treated Ti-6Al-4V-Ca2+/Pi surface induces osteoblast differentiation by regulating the expression of DMP1 and IFITM5. Therefore, surface microstructure modification through PEO coatings with Ca2+/Pi ions could be used as a valuable method to improve biocompatibility properties of titanium alloys.

Formation of nano-phase hydroxyapatite film on TiO2 nano-network.

Nano- and micro-phase HA film formed on TiO2 nano-network surface by simple electrochemical treatment. The range of lateral pore size of the network specimen was about 10-120 nm on Ti surface by anodized in 5 M NaOH solution at 0.3 A for 10 min. Nano-network TiO2 surface were formed by this anodization step which acted as templates and anchorage for growth of the HA during subsequent pulsed electrochemical deposition process at 85 degrees C. The phase and morphologies of deposits HA were influenced by the electrolyte concentration. The nano needle-like precipitates formed under low SBF concentration were identified to be HA crystals orientated parallel to the c-axis direction. Increasing electrolyte concentration, needle-like deposits transferred to the plate-like and micro plate like precipitates in the case of high SBF concentration.