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In this study, the effect of the applied potential on nano-particle formation during plasma electrolytic oxidation (PEO) was investigated. A Ti-6Al-4 V ELI disk was used as the substrate for PEO. Using a pulsed DC power supply, voltages of 180, 280, and 380 V were applied for 3 min to the substrate in an electrolyte containing an aqueous solution of Ca and P. The morphology and crystalline structure of the PEO-treated surface were studied using X-ray diffraction, field-emission scanning electron microscopy, and nanoindentation testing. When the lowest voltage was applied, some partially formed pores were observed on the PEO-treated surface. With increasing applied voltage, larger and more uniform pores were formed. However, when the voltage was too high, cracks appeared around the formed pores. The crystallite size also increased with an increase in the applied voltage; however, microcracks were generated on the PEO surface when the applied voltage exceeded a certain value. [ABSTRACT FROM AUTHOR]

Surface modification of dental implants or orthopedic implants is important for biocompatibility, and Ti-6Al-4 V alloy is mainly used as implant material for clinical use. In particular, research on the formation of nanotubes for drug doping to improve biocompatibility is in progress. For the control of nanotube shape, in this study, nanotube shape changes on Ti-6Al-4 V alloy via various applied potential for bio-implants were researched using various instruments. The formation of nanotubes on the surface of the Ti-6Al-4 V alloy was performed using a DC power source as a two-electrode system, and platinum as a counter electrode and a working electrode as an anode. The electrolyte was 0.8 wt. % NaF solution and 1.0 M H3PO4 were used and mixed using a magnetic bar during anodization. At this time, the voltage applied when forming the nanotubes was varied as (10 → 20 → 30 V), (30 → 10 → 30 V), and (10 → 30 → 30 V), respectively, and these voltages were applied for 30 min for each step. After the formation of nanotubes, the surface morphology and structural properties of the samples were observed using field-emission scanning electron microscope, X-ray diffractometer, Fourier transform infrared spectroscopy, and nanoindentation tester. The higher the voltage applied during the formation of nanotubes, the larger is the diameter. In the case of the nanotube (10 → 20 → 30 V), the top of the nanotube was narrow and the diameter increased toward the bottom, forming a cone shape. In the case of the nanotube (30 → 10 → 30 V), a narrow waist shape was formed, and in the case of the nanotube (10 → 30 → 30 V), a jar shape was formed with anatase and rutile phases. From the FT-IR results, when nanotubes are formed, TiO2 anatase was detected and showed the tendency to change from crystallization to amorphous state. The indentation hardness and elastic modulus decreased for the nanotube surface compared with those of the bulk Ti alloy. [ABSTRACT FROM AUTHOR]

In general, Ti alloys are commonly used as biomaterials for implants. However, in the case of such alloys, the high elastic modulus causes stress shielding effects and bacterial growth, reducing their biocompatibility. In order to improve it, new alloys composed of Ti–Nb–Ag–Pt were developed in this study because it is possible to reduce the elastic modulus by adding an alloying element, such as Nb, and to reduce the bacterial activity by adding Ag and Pt elements. The following studies were conducted with the aim of manufacturing and forming nanotubes on the surface to greatly improve the biocompatibility. Ti–xNb–Ag–Pt alloys were manufactured using a vacuum arc furnace in an Ar atmosphere, homogenized for 1 h at 1050 °C, and then quenched at 0 °C. The formation of nanotubes on the surfaces of the alloys was performed using the anodization method with an applied voltage of 30 V in 1 M H3PO4 + 0.8 wt% NaF for 1 h at 25 °C. The formed nanotube surfaces were analyzed by optical microscopy, field emission scanning electron microscopy, X-ray diffraction, energy-dispersive X-ray spectroscopy, nanoindentation tests, and antibacterial tests. Antibacterial activity was evaluated according to the ISO 22196:2007 method, for which S. aureus (NBRC122135) was used. The microstructure of Ti–10Nb–Ag–Pt was a needle-like structure, and Ti–50Nb–Ag–Pt presented both an equiaxed structure and a needle-like structure. The size of the nanotube diameter decreased as the Nb content increased. The Ag and Pt elements were evenly distributed on the nanotube-formed alloy surfaces. The Vickers hardness and the elastic modulus value decreased as the Nb content increased. Following the nanotube formation, the Vickers hardness and elastic modulus values decreased by thrice, and only the nanotube-formed Ti–xNb alloys containing Ag and Pt showed the antibacterial activity effect. [ABSTRACT FROM AUTHOR]

ABSTRACT The phenomena of hydroxyapatite (HA) precipitation in micropore-structured Ti alloy have been studied using transmission electron microscopy and field-emission SEM (FE-SEM). HA layer was grown on anodized Ti surface by electrochemical deposition process in modified simulated body fluid at 85 °C. The deposition process involved two steps: (i) porous TiO2 on Ti alloy was formed at high potential, and (ii) cyclic voltammetric method was carried out in modified simulated body fluid for HA electrodeposition on anodized Ti alloys. Homogenized Ti-30Nb alloy showed the equiaxed structure with β phase, whereas the Ti-30Ta alloy showed the martensite structure with α″ phase. In case of anodized Ti binary alloys at applied 270 V, the anodized surface showed the uniform pore formation and Ca/P ratio was the range of 1.61 and 1.72. HA was formed with plate and fiberlike shape on anodized Ti alloys. HA was precipitated densely in the pore and connected with each other in the TiO2 layer. The selected-area diffraction patterns of the HA were composed of rings and intense spots with some crystallized precipitates. Copyright © 2012 John Wiley & Sons, Ltd. [ABSTRACT FROM AUTHOR]

ABSTRACT Nanotube growth analysis in the interface between oxide film and titanium alloy substrate has been researched using scanning transmission electron microscope and field-emission scanning electron microscopy (FE-SEM). The Ti-35Nb-xHf (x =3, 7 and 15 wt.%) alloys were prepared using the sponges of Ti, Nb and Hf. The nanotube on the alloy surface was formed in 1.0 M H3PO4 with 0.8 wt.% NaF, using a potentiostat. The nanotube growth analysis on the titanium alloys was investigated using FE-SEM, energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy and X-ray diffraction. Microstructures of Ti-35Nb-xHf alloys showed an equiaxed structure and the α' phase decreased with Hf content, whereas the β phase increased as Hf content increased. The nanotube surface mainly consisted of Nb and Ti oxide. The peaks of Nb and O elements exhibited higher intensities on the nanotube surface compared with the matrix, whereas peaks of Ti and Hf exhibited lower intensities on the matrix surface from EDS line profile. The shape of nanotube on the Ti-35Nb-xHf showed two scales of nanotubes; large (190 nm-220 nm) and small (91 nm-104 nm). The diameter of the nanotubes decreased with increasing the Hf content, whereas the length of the nanotubes increased with increasing Hf content. Copyright © 2012 John Wiley & Sons, Ltd. [ABSTRACT FROM AUTHOR]

The measurement of oxide thin film dissolution rate on the hydroxyapatite (HA)-coated Ti alloy was researched by scanning electron microscopy and impedance spectroscopy. For this study, Ti-35Nb-xHf alloys containing Hf from 3 wt.% to 15 wt.% were manufactured by using a vacuum furnace system. Ti-35Nb-xHf alloys were homogenized for 24 h at 1000 °C. HA thin films for applications in the bio-medical field were grown by radio-frequency (RF) magnetron sputtering techniques. RF power of 50 W was applied to the target for 1 h at 100 °C. The microstructure, phase, and composition of HA-coated Ti-35Nb-xHf alloys were examined by field-emission scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction. The estimation of corrosion behavior was performed by potentiodynamic and alternating current impedance test. The experimental results indicated that the as-sputtered coating had quite uniform thickness and well bonded to the substrate. The HA film on the Ti-35Nb-xHf alloys exhibited a better electrochemical behavior than bared Ti-35Nb-xHf alloys in the passive region. The high capacity behavior (constant phase element) was observed for HA-coated Ti-35Nb-15Hf alloy, and the polarization resistance (Rp) of HA-coated Ti-35Nb-xHf alloys was higher than that of uncoated Ti-35Nb-xHf alloys. Copyright © 2012 John Wiley & Sons, Ltd. [ABSTRACT FROM AUTHOR]

The purpose of this study was to investigate the mechanisms involved in the failure of magnetic attachments used to retain dental prostheses. Dyna magnets were retrieved from dentures that had failed after 34 months of clinical use. These magnetic attachments were prepared and sectioned so as to observe the corrosion surface and layer in order to analyze the corrosion behaviors of the attachments. The corroded surface was observed under a field emission scanning electron microscope (FE-SEM) (JSM 840A, JEOL, Japan). An X-ray diffractometer (XRD) was used to analyze the corrosion product formed due to corrosion in the oral environment. Erosion-corrosion started in the uneven portion of the stainless steel cover in the magnetic attachments composed with Nd−Fe−B alloy. Corrosion was initiated on the worn stainless steel surface, followed by spalling of magnetic material due to corrosive solution. The corrosion rate increased drastically after the corrosion product caused spalling in Nd−Fe−B alloy. Corrosion initiated in the uneven stainless steel surface as well as in the welded zone. In conclusion, the failure of magnetic attachments may occur by either welding failure or breakdown of the encapsulating material. Thus, we believe that treating the surface of magnetic attachments would resolve the corrosion problem seen in magnetic attachments to some extent. [ABSTRACT FROM AUTHOR]

In order to study the electrochemical behaviors of TiN film coated Ti−Nb alloys for dental materials, Ti containing Nb up to 3, 20, and 40 wt.% was melted by a vacuum furnace and coated with TiN by EB-PVD. the electrochemical behaviors were investigated using a potentiostat in 0.9% NaCl solution and the corrosion surface was observed using SEM and XPS. Ti−3Nb and Ti−20Nb alloys have α+β phase structure. In the case of Ti−40Nb, the microstructure had a coarse β phase. The microstructural changed from equiaxed to acicular and an increase of β-phase in Ti−Nb alloys was observed with increased Nb content. The current density at 300 mV (potential of oral environment) of Ti−40Nb alloy was lower than that of the other alloys in 0.9% NaCl. The pitting corrosion resistance of Ti−40Nb was higher than that of Ti−3Nb and Ti−20Nb alloys in the 0.9% NaCl solution. The corrosion potential and pitting potential of TiN coated Ti alloy increased with increasing Nb content but the current density at 300 mV and the current density at the passive region decreased. The TiN coated Ti−40Nb alloy offers good corrosion resistance for dental implants compared with non-TiN coats alloys. [ABSTRACT FROM AUTHOR]

Interface activation and surface characteristics of Ti/TiN/HA film coated sintered stainless steels (SSS) have been investigated by electrochemical and biocompatibility tests. HA (hydroxyapatite), Ti, and Ti/TiN film coatings were applied using electron-beam deposition method (EB-PVD). Ti, Ti/TiN, and Ti/TiN/HA film coated surfaces and layers were investigated by SEM and XPS. The coated films showed micro-columnar structure, and Ti/TiN/HA films were denser than Ti or HA-only film. The corrosion resistance of the HA coating was similar to that of Ti/TiN/HA film coating when Cu content reached 4 wt.%, but the corrosion resistance of the HA coating decreased when Cu content increased from 4 wt.% in 0.9% NaCl solution. Therefore, HA-only coating could ensure corrosion resistance when Cu content does not exceed 4 wt.%. The results of biocompatibility tests of SSS on dogs showed that bone formation and biocompatibility were favorable when Cu content did not exceed 4 wt.%. The biocompatibility with bone was generally favorable in Ti/TiN/HA film coating and HA-only coating, while bone formation was somewhat faster for the HA film coated surface than for the Ti/TiN/HA film coating. Also, good cell growth and osseointegration without toxicity were observed. [ABSTRACT FROM AUTHOR]

Surface alteration of implant screws after function may be associated with mechanicalffailure. This type of metal fatigue appears to be the most common cause of structural failure. The purpose of this study was to evaluate surface alteration of implant screws after function through an examination of used and unused implant screws via scanning electron microscopy (SEM). In this study, abutment screws (Steri-oss, 3i, USA), gold retaining screws (3i, USA), and titanium retaining screws (3i, USA) were retrieved from patients, New, unused abutment, and retaining screws were prepared for a control group. Each of the old, used screws was retrieved with a screwdriver. The retrieved implant complex of a Steri-oss system was also prepared for this study. SEM investigation and energy dispersive spectroscopy (EDS) analysis of the abutment and retaining screws were then performed, as well as SEM investigation of a cross-sectioned sample of the retrieved implant complex in the case of new, unused implant screws, as-manufactured circumferential grooves were regularly examined and screw threads were sharply maintained. Before ultrasonic cleansing of old, used implant screws, there was a large amount of debris accumulation and corrosion products. After ultrasonic cleansing of old, used implant screws, circumferential grooves were examined were found to be randomly deepened and scratching increased. Also, dull screw fhreads were observed. More surface alterations after function were observed in titanium screws than in gold screws. Furthermore, more surface alteration was observed when the screws were retrieved with a driver than without a driver. These surface alterations after function may result in screw instability. Regular cleansing and exchange of screws is therefore recommended. We also recommend the use of gold screws over titanium screws, and careful manipulation of the driver. [ABSTRACT FROM AUTHOR]

Regardless of the type of performed restoration, in most cases, a screw connection is employed between the abutment and implant. For this reason, implant screw loosening has remained a problem in restorative practices. The purpose of this study was to compare the surface of coated/plated screws with titanium and gold alloy screws and to evaluate the physical properties of coated/plated material after scratch tests via FE-SEM (field emission scanning electron microscopy) investigation. GoldTite, titanium screws provided by 3i (Implant Innovation, USA) and TorqTite, titanium screws by Steri-Oss (Nobel Biocare, USA) and gold screws and titanium screws by AVANA (Osstem Implant, Korea) were selected for this study. The surface, crest, and root of the abutment screws were observed by FE-SEM. A micro-diamond needle was also prepared for the scratch test. Each abutment screw was fixed, and a scratch on the surface of the head region was made at constant load and thereafter the fine trace was observed with FE-SEM. The surface of GoldTite was smoother than that of other screws and it also had abundant ductility and malleability compared with titanium and gold screws. The scratch tests also revealed that teflon particles were exfoliated easily in the screw coated with teflon. The titanium screw had rough surface and low ductility. The clinical use of gold-plated screws is recommended as a means of preventing screw loosening. [ABSTRACT FROM AUTHOR]

Although fortunately rare, fracture of implants causes significant problems for both clinicians and patients. The major cause of a fractured implant may be corrosion fatigue fracture. To investigate how to increase the fatigue life and corrosion resistance of dental implants, the surface morphology of six Steri-Oss fractured implants was analyzed. The period of implantation after loading in patient jaws varied between 23 months and 37 months. The topography and surface chemical composition were studied with electron probe micro-analysis (point mapping, energy dispersive x-ray spectroscopy) and field emission scanning electron microscopy. All samples were fractured at the screw root and the crest formed a keen-edged shape. The five samples were fractured at the first thread of the fixture and one sample at the third thread of fixture. The fatigue cracks were mainly nucleated and grown at scratches occurring for the screw root and crest formation and the cervix portion of the implant having a small curvature. The pits were nucleated in the vicinity of inclusions such as SiO2 and corrosion fatigue cracking was predominantly propagated. Corrosion products were found on the opposite side of the starting point of corrosion fatigue crack. From observations of fatigue striations, it is possible to predict the life time of fractured implants and estimate the cleavage fracture and dimple fracture of implants. In this study, analysis of fractured surfaces revealed the characteristics of the implant materials, problems of design, fatigue life, and manufacturing process. In order to protect against corrosion fatigue fractures and prolong the fatigue life of dental implants, we must consider the implant design, implant manufacturing, and surface treatment of the implant materials. [ABSTRACT FROM AUTHOR]

Two types of HL hexed abutments of a Steri-Oss system, gold/plastic coping and gold coping, were compared in terms of corrosion behavior. The anodic polarization behavior and the galvanic corrosion between abutments and Type III gold alloys, before and after casting, were analyzed. In addition, the crevice corrosion of the casting samples was analyzed with cyclic potentiodynamic polarization tests using the |Er-Ecorr| value and scanning electron microscopy. Before casting, gold/plastic coping and gold coping were shown to have similar corrosion patterns in the anodic polarization test. Type III casting gold alloy was shown to have a lower higher than that of gold coping, but the passive region for the gold/plastic coping was smaller than that of gold coping. The contact current density between the cast gold alloys and gold/plastic before casting was higher than that between gold coping and cast gold alloy. The contact current density of the samples after casting was shown to be similar to that before casting. The crevice corrosion resistance of cast samples using gold coping was lower than that of cast samples using gold/plastic coping, and severe corrosion was observed by SEM at the abutment-casting gold alloy interface. [ABSTRACT FROM AUTHOR]

The present study examined the in vitro and in vivo bone formation and adhesion ability on the surface of a titanium dental implant made by plasma electrolytic oxidation (PEO) in electrolytes containing bioactive ions. To achieve this goal, screw-shaped fabricated Ti-6Al-4V alloy implants were processed via PEO using an electrolyte solution containing calcium (Ca), phosphorous (P), magnesium (Mg), zinc (Zn), strontium (Sr), silicon (Si), and manganese (Mn) species. The screw implants doped with bioactive elements via PEO were placed in rabbit tibia, and the results were compared to the sand-blasted Ti-6Al-4V alloy implants. At eight-week post-surgery, there was no significant difference in the values of removal torque between sand-blasted and PEO-treated implants. However, it was observed that the PEO treatment of dental implants led to the formation of more periphery bone as compared to the case of sand-blasted implants. Accordingly, the PEO-treated implants have the potential to be used as promising materials for dental applications. [ABSTRACT FROM AUTHOR]

In this study, we investigated the electrochemical characteristics of TiN/ZrN multilayers on a Ti–35Ta–xHf alloy by radio frequency (RF) magnetron sputtering. The Ti–35Ta–xHf alloy had an α''+ β phase structure. The Ti–35Ta–15Hf alloy had a higher intensity β phase peak than Ti–35Ta–3Hf and 7Hf alloy, which contained lower Hf content. The martensite traces disappeared with increasing Hf content and the Ti–35Ta–15Hf alloy showed an entirely equiaxed structure with a β phase. The multilayer film was developed by alternately depositing TiN and ZrN layers on Ti–35Ta–15Hf substrates using the RF magnetron sputtering system to improve the interface properties between the coating and substrate. The uncoated specimen showed a passive region between 60 and 1300 mV with a current density of 0.38 µA/cm2, whereas, the TiN/ZrN multilayered specimen had a passive region between 210 and 1500 mV with a current density of 0.09 µA/cm2. The experimental results suggest that the as-sputtered layer coated well on the substrate. The TiN/ZrN multilayered film on Ti–35Ta–15Hf substrate exhibited better electrochemical resistance than that of the uncoated Ti–35Ta–15Hf substrate. [ABSTRACT FROM AUTHOR]