• The Journal of Korean Academy of Prosthodontics
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• v.51 no.4
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• pp.261-268
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• 2013

Purpose: The purpose of this study was to investigate the effect of geometrically different wax pattern shapes and sizes on the castability of Grade2 Cp-Ti (commercially pure titanium). Materials and methods: Total of 40 mesh wax pattern ($61mm{\times}24mm$, 207 grids), ($61mm{\times}17mm$, 138 grids) was cast in this experiment. Depending on the geometrical shape of the wax pattern, 8 groups was organized; Flat, Semicircular, Horse-shoe and V-shape, each consisting 5 samples. Runner-bar sprue was used in all patterns. The number of completely cast grid in wax pattern served as a measure for the castability of comercially pure titanium. Results: The mean value of square count in each group was as followed; 133.20 squares in group SS (96.52%), 132.40 squares in group SH (95.94%), 132.00 squares in group SF (95.65%), 127.60 squares in SV (91.43%), 198.60 squares in group LF (95.94%), 197.80 squares in group LV (95.56%), 196.40 squares in group LS (94.88%), and 188.00 squares in group LH (90.82%). Conclusion: Within the limitations of this study the results indicate that there were no sttistically significant difference in castability of titanium regarding wax pattern shape (P>.05). However, Small size wax patterns were showing the noticeable castability more than Large size pattern.

• The Journal of Korean Academy of Prosthodontics
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• v.45 no.1
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• pp.85-97
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• 2007

Statement of problem: Recently, anodic oxidation of cp-titanium is a popular method for treatment of titanium implant surfaces. It is a relatively easy process, and the thickness, structure, composition, and the microstructure of the oxide layer can be variably modified. Moreover the biological properties of the oxide layer can be controlled. Purpose: In this study, the roughness, microstructure, crystal structure of the variously treated groups (current, voltage, frequency, electrolyte, thermal treatment) were evaluated. And the specimens were soaked in simulated body fluid (SBF) to evaluate the effects of the surface characteristics and the oxide layers on the bioactivity of the specimens which were directly related to bone formation and integration. Materials and methods: Surface treatments consisted of either anodization or anodization followed thermal treatment. Specimens were divided into seven groups, depending on their anodizing treatment conditions: constant current mode (350V for group 2), constant voltage mode (155V for group 3), 60 Hz pulse series (230V for group 4, 300V for group 5), and 1000 Hz pulse series (400V for group 6, 460V for group 7). Non-treated native surfaces were used as controls (group 1). In addition, for the purpose of evaluating the effects of thermal treatment, each group was heat treated by elevating the temperature by $5^{\circ}C$ per minute until $600^{\circ}C$ for 1 hour, and then bench cured. Using scanning electron microscope (SEM), porous oxide layers were observed on treated surfaces. The crystal structures and phases of titania were identified by thin-film x-ray diffractmeter (TF-XRD). Atomic force microscope (AFM) was used for roughness measurement (Sa, Sq). To evaluate bioactivity of modified titanium surfaces, each group was soaked in SBF for 168 hours (1 week), and then changed surface characteristics were analyzed by SEM and TF-XRD. Results: On basis of our findings, we concluded the following results. 1. Most groups showed morphologically porous structures. Except group 2, all groups showed fine to coarse convex structures, and the groups with superior quantity of oxide products showed superior morphology. 2. As a result of combined anodization and thermal treatment, there were no effects on composition of crystalline structure. But, heat treatment influenced the quantity of formation of the oxide products (rutile / anatase). 3. Roughness decreased in the order of groups 7,5,2,3,6,4,1 and there was statistical difference between group 7 and the others (p<0.05), but group 7 did not show any bioactivity within a week. 4. In groups that implanted ions (Ca/P) on the oxide layer through current and voltage control, showed superior morphology, and oxide products, but did not express any bioactivity within a week. 5. In group 3, the oxide layer was uniformly organized with rutile, with almost no titanium peak. And there were abnormally more [101] orientations of rutile crystalline structure, and bonelike apatite formation could be seen around these crystalline structures. Conclusion: As a result of control of various factors in anodization (current, voltage, frequency, electrolytes, thermal treatment), the surface morphology, micro-porosity, the 2nd phase formation, crystalline structure, thickness of the oxide layer could be modified. And even more, the bioactivity of the specimens in vitro could be induced. Thus anodic oxidation can be considered as an excellent surface treatment method that will able to not only control the physical properties but enhance the biological characteristics of the oxide layer. Furthermore, it is recommended in near future animal research to prove these results.

• The Journal of Korean Academy of Prosthodontics
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• v.49 no.1
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• pp.65-72
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• 2011

Purpose: The purpose of this study was to evaluate the level of electro-chemical corrosion and surface roughness change for the cases of Ti abutment connected to restoration made of base metal alloys. Materials and methods: It was hypothesized that Ni-Cr alloys in different compositions possess different corrosion resistances, and thus the specimens ($13{\times}13{\times}1.5\;mm$) in this study were fabricated with 3 different types of metal alloys, commonly used for metal ceramic restorations. The electrochemical characteristics were evaluated with potentiostat (Parstat 2273A) and the level of surface roughness change was observed with surface roughness tester. Paired t-test was used to compare mean average surface roughness (Ra) changes of each specimen group. Results: All specimens made of nickel-chromium based alloys, average surface roughness was increased significantly (P < .05). Among them, the Ni-Cr-Be alloy ($0.016{\pm}.007\;{\mu}m$) had the largest change of roughness followed by Ni-Cr ($0.012{\pm}.003\;{\mu}m$) and Ni-Cr-Ti ($0.012{\pm}.002\;{\mu}m$) alloy. There was no significant changes in surface roughness between each metal alloys after corrosion. Conclusion: In the case of galvanic couples of Ti in contact with all specimens made of nickel-chromium based alloys, average surface roughness was increased.

• Journal of Korean Dental Science
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• v.10 no.1
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• pp.10-21
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• 2017

Purpose: The purpose of this study was to investigate the electrochemical characteristics of nanotubular Ti-25Nb-xZr ternary alloys for dental implant materials. Materials and Methods: Ti-25Nb-xZr alloys with different Zr contents (0, 3, 7, and 15 wt.%) were manufactured using commercially pure titanium (CP-Ti), niobium (Nb), and zirconium (Zr) (99.95 wt.% purity). The alloys were prepared by arc melting in argon (Ar) atmosphere. The Ti-25Nb-xZr alloys were homogenized in Ar atmosphere at $1,000^{\circ}C$ for 12 hours followed by quenching into ice water. The microstructure of the Ti-25Nb-xZr alloys was examined by a field emission scanning electron microscope. The phases in the alloys were identified by an X-ray diffractometer. The chemical composition of the nanotube-formed surfaces was determined by energy-dispersive X-ray spectroscopy. Self-organized $TiO_2$ was prepared by electrochemical oxidation of the samples in a $1.0M\;H_3PO_4+0.8wt.%$ NaF electrolyte. The anodization potential was 30 V and time was 1 hour by DC supplier. Surface wettability was evaluated for both the metallographically polished and nanotube-formed surfaces using a contact-angle goniometer. The corrosion properties of the specimens were investigated using a 0.9 wt.% aqueous solution of NaCl at $36^{\circ}C{\pm}5^{\circ}C$ using a potentiodynamic polarization test. Result: Needle-like structure of Ti-25Nb-xZr alloys was transform to equiaxed structure as Zr content increased. Nanotube formed on Ti-25Nb-xZr alloys show two sizes of nanotube structure. The diameters of the large tubes decreased and small tubes increased as Zr content increased. The lower contact angles for nanotube formed Ti-25NbxZr alloys surfaces showed compare to non-nanotube formed surface. The corrosion resistance of alloy increased as Zr content increased, and nanotube formed surface showed longer the passive regions compared to non-treatment surface. Conclusion: It is confirmed that corrosion resistance of alloy increased as Zr content increased, and nanotube formed surface has longer passive region compared to without treatment surface.

• The Journal of Korean Academy of Prosthodontics
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• v.39 no.1
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• pp.71-83
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• 2001

The purpose of this study was to compare the effects of various surface treatments by measuring removal torque on bone healing around titanium implants. 40 Screw-shaped cp titanium implants with length of 4mm, outer diameter of 3.75mm, and pitch-height of 0.5mm were used Group 1 was left as machined(control), Group 2 was blasted with $50{\mu}m\;Al_2O_3$, group 3 was blasted and etched in etching solution($NH_4OH : H_2O_2:H_2O= 1 : 1 : 5$) at $90^{\circ}C$ for 1 minute group 4 was blasted and oxidated under pure oxygen at $800^{\circ}C$. The implant surface roughness was analyzed with SEM and CLSM(Confocal Laser Scanning Microscope) and implants were placed in proximal tibial metaphysis of 10 New Zealand White rabbits. After 3 months of healing period, removal torque of each implant was measured to compare bone healing around implant. The results obtained were as follows 1. In SEM view, blasting increased the roughness of the surface, but etching of that rough surface decreased the roughness due to the removal of the tip of the peak. Oxidation also decreased the roughness due to formation of needle-like oxide grains on the implant surface. 2. The Sa value from CLSM was least in the machined group($0.47{\mu}m$), greatest in blasted group($1.25{\mu}m$), and the value decreased after etching($0.91{\mu}m$) and oxidation($0.94{\mu}m$). 3. The removal torque of etched group(24.5Ncm) was greater than that of machined group(16.7Ncm) (P<0.05), and was greatest in the oxidated group(40.3Ncm) and the blasted group(34.7Ncm).

• Journal of the Korean Society for Heat Treatment
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• v.18 no.2
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• pp.91-98
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• 2005

Both commercially pure titanium and Ti-6Al-4V alloy have been widely used as biomaterials because of their excellent biocompatibility, corrosion resistance and mechanical properties. However, in recent years, vanadium has been found to cause cytotoxic effects and adverse tissue reactions, while aluminium has been associated with potential neurological disorders. A newly designed ${\alpha}+{\beta}$ type Ti alloy, Ti-10Ta-10Nb alloy showed superior properties to CP Ti and Ti-6Al-4V alloy in the point of biomaterial, and elucidated the future uses as a biomaterial. Microstructural changes of Ti-10Ta-10Nb alloy after hot-rolling, warm-rolling, solution and aging treatment were investigated. According to TEM results, the microstructures after solution treatment were composed of mostly ${\alpha}$ phase with a trace of ${\beta}$ phase due to adding ${\beta}$-phase stabilizer tantalum and niobium. The microstructures after warm-rolling is coarse and elongated ${\alpha}$ phase and hot rolling resulted in very fine ${\alpha}$ widmanst$\ddot{a}$tten. The highest value of hardness was obtained by aging treatment at $400^{\circ}C$ for 20hr in which microstructure consisted of very fine ${\alpha}$ phase in ${\beta}$ matrix.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.198-198
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• 2016

An ideal orthopedic implant should provide an excellent bone-implant connection, less implant loosening and minimum adverse reactions. Commercial pure titanium (CP-Ti) and Ti alloys have been widely utilized for biomedical applications such as orthopedic and dental implants. However, being bioinert, the integration of such implant in bone was not in good condition to achieve improved osseointegraiton, there have been many efforts to modify the composition and topography of implant surface. These processes are generally classified as physical, chemical, and electrochemical methods. Plasma electrolytic oxidation (PEO) as an electrochemical route has been recently utilized to produce this kind of composite coatings. Mg ion plays a key role in bone metabolism, since it influences osteoblast and osteoclast activity. From previous studies, it has been found that Mg ions improve the bone formation on Ti alloys. PEO is a promising technology to produce porous and firmly adherent inorganic Mg containing $TiO_2$($Mg-TiO_2$ ) coatings on Ti surface, and the amount of Mg introduced into the coatings can be optimized by altering the electrolyte composition. In this study, a series of $Mg-TiO_2$ coatings are produced on Ti-6Al-4V ELI dental implant using PEO, with the substitution degree, respectively, at 0, 5, 10 and 20%. Based on the preliminary analysis of the coating structure, composition and morphology, a bone like apatite formation model is used to evaluate the in vitro biological responses at the bone-implant interface. The enhancement of the bone like apatite forming ability arises from $Mg-TiO_2$ surface, which has formed the reduction of the Mg ions. The promising results successfully demonstrate the immense potential of $Mg-TiO_2$ coatings in dental and biomaterials applications.

• The Journal of Korean Academy of Prosthodontics
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• v.48 no.4
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• pp.308-314
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• 2010

Purpose: The purpose of this study is to analyze the change in re-osseointegration over time and bone reaction at the interface between implant fixture and the surface of the bone, after destroying re-osseointegration by distorting the bone-implant interface artificially. Materials and methods: Experimental implant fixtures (cp titanium, ${\phi}3.75\;mm{\times}4\;mm$) which didn't have surface treatment were produced. Two or three fixtures were implanted on both tibias of twelve female rabbits (New Zealand white, more than 3.5 kg). Then after six weeks, removal torque (RT) was measured and the results were recorded as the first measurement values. The fixtures were submerged again to get reosseointegration between the bone and fixture. To identify the change in re-osseointegration of submerged fixtures over time, six groups had the healing time for four days (group I), one week (group II), two weeks (group III), three weeks (group IV), four weeks (group V) and five weeks (group VI), and then the secondary removal torque was measured for each group. To identify the bone formation under fluorescent light, tetracycline (15 mg/kg, IM) were treated on the rabbits of each group. After the second measurement, the rabbits were sacrificed, and 16 slides were made, two or three for each group. The slides were observed under the fluorescent light with light microscope. To find out the change in the secondary removal torque over the primary removal torque in progress of time, the averages of the increase rate of the primary and secondary torque removal force were calculated. Then, to find out if there were any critical differences between the primary removal torque and the secondary removal torque in each group and among the groups, the results were analyzed statistically by paired t- test, one-way ANOVA, and Duncan's Multiple Range Test. Results: In group I and II, secondary removal torque decreased, especially in group I. In group III, IV, V, and VI, secondary removal torque increased critically. Comparing the differences among the groups, the critical difference was shown between group I, II and group III, IV, V, VI. Mineralization at the interface between the bone and implant fixture was identified from the first week, and bone formation was shown more clearly from the second week. Conclusion: If the implant fixture remains unforced for a certain period of time after the fixture has had iatrogenic mobility, re-osseointegration occurs at the surface of the fixture, and for tibias of rabbits, higher re-osseointegration was obtained within two weeks.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.197-197
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• 2016

Commercially pure titanium (CP Ti) and Ti-6Al-4V alloys have been widely used for biomedical applications. However, the use of the Ti-6Al-4V alloy in biomaterial is then a subject of controversy because aluminum ions and vanadium oxide have potential detrimental influence on the human body due to vanadium and aluminum. Hence, recent works showed that the synthesis of new Ti-based alloys for implant application involves more biocompatible metallic alloying element, such as, Nb, Hf, Zr and Mo. In particular, Nb and Hf are one of the most effective Ti ${\beta}-stabilizer$ and reducing the elastic modulus. Plasma electrolyte oxidation (PEO) is known as excellent method in the biocompatibility of biomaterial due to quickly coating time and controlled coating condition. The anodized oxide layer and diameter modulation of Ti alloys can be obtained function of improvement of cell adhesion. Manganese(Mn) plays very important roles in essential for normal growth and metabolism of skeletal tissue in vertebrates and can be detected as minor constituents in teeth and bone. Radio frequency(RF) magnetron sputtering in the various PVD methods has high deposition rates, high-purity films, extremely high adhesion of films, and excellent uniform layers for depositing a wide range of materials, including metals, alloys and ceramics like a hydroxyapatite. The aim of this study is to research the Mn coatings on the micro-pore formed Ti-29Nb-xHf alloys by RF-magnetron sputtering for dental applications. Ti-29Nb-xHf (x= 0, 3, 7 and 15wt%, mass fraction) alloys were prepared Ti-29Nb-xHf alloys of containing Hf up from 0 wt% to 15 wt% were melted by using a vacuum furnace. Ti-29Nb-xHf alloys were homogenized for 2 hr at $1050^{\circ}C$. Each alloy was anodized in solution containing typically 0.15 M calcium acetate monohydrate + 0.02 M calcium glycerophosphate at room temperature. A direct current power source was used for the process of anodization. Anodized alloys was prepared using 270V~300V anodization voltage at room. Mn coatings was produced by RF-magnetron sputtering system. RF power of 100W was applied to the target for 1h at room temperature. The microstructure, phase and composition of Mn coated oxide surface of Ti-29Nb-xHf alloys were examined by FE-SEM, EDS, and XRD.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.199-199
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• 2016

Commercially pure titanium (cp-Ti) and Ti alloys (typically Ti-6Al-4V) display excellent corrosion resistance and biocompatibility. Although the chemical composition and topography are considered important, the mechanical properties of the material and the loading conditions in the host have, conventionally. Ti and its alloys are not bioactive. Therefore, they do not chemically bond to the bone, whereas they physically bond with bone tissue. The electrochemical deposition process provides an effective surface for biocompatibility because large surface area can be served to cell proliferation. Electrochemical deposition method is an attractive technique for the deposition of hydroxyapatite (HAp). However, the adhesions of these coatings to the Ti surface needs to be improved for clinical used. Plasma electrolyte oxidation (PEO) enables control in the chemical com position, porous structure, and thickness of the $TiO_2$ layer on Ti surface. In addition, previous studies h ave concluded that the presence of $Ca^{+2}$ and ${PO_4}^{3-}$ ion coating on porous $TiO_2$ surface induced adhesion strength between HAp and Ti surface during electrochemical deposition. Silicon (Si) in particular has been found to be essential for normal bone and cartilage growth and development. Zinc (Zn) plays very important roles in bone formation and immune system regulation, and is also the most abundant trace element in bone. The objective of this work was to study electrochemical characteristcs of Zn and Si coating on Ti-6Al-4V by PEO treatment. The coating process involves two steps: 1) formation of porous $TiO_2$ on Ti-6Al-4V at high potential. A pulsed DC power supply was employed. 2) Electrochemical tests were carried out using potentiodynamic and AC impedance methoeds. The morphology, the chemical composition, and the micro-structure an alysis of the sample were examined using FE-SEM, EDS, and XRD. The enhancements of the HAp forming ability arise from $Si/Zn-TiO_2$ surface, which has formed the reduction of the Si/Zn ions. The promising results successfully demonstrate the immense potential of $Si/Zn-TiO_2$ coatings in dental and biomaterials applications.