• 한국재료학회지
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• 제14권3호
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• pp.211-217
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• 2004

The oxidation behaviors of Ti-10Ta-10Nb alloy and Ti-6Al-4V alloy were studied in dry air atmosphere. Specimens were melted in consumable vacuum arc furnace and homogenized at $1050^{\circ}C$ for 24 h. Hot rolling was performed at $1000^{\circ}C$. Specimens of the alloys were oxidized as the temperature range $400~650^{\circ}C$ for 30 min. The oxidation behavior of the alloys was analysed by optical microscope, SEM/EDX, XRD, XPS and TGA. Immersion test was performed in 1% Lactic acid. In the microscope observation, oxide layer of Ti-10Ta-10Nb alloy was denser and thinner than Ti-6Al-4V's. The weight gains during the oxidation rapidly increased at the temperature above $600^{\circ}C$ in Ti-6Al-4V's alloy and$ 700^{\circ}C$ in Ti-10Ta-10Nb alloy. According to XRD results, oxide layers were composed of mostly $TiO_2$(rutile) phase. It was analysed that the passive film of the Ti alloys consisted of $TiO_2$ through X-ray photoelectron spectroscopy(XPS) analysis.

• 대한치과기공학회지
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• 제26권1호
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• pp.139-144
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• 2004

In the present study, a simple method was successfully used for hydroxyapatite coatings on Ti-6Al-4V substrates deposited by using a sol-gel derived precursor. Prior to hydroxyapatite coating the samples were micropolished (0.1 micron) and divided into three sets. The first set,were the micropolished samples kept as such. The second set were coated with titania sol and the third set was treated with 5M NaOH. After three repetitions of hydroxyapatite coating procedures on each set and heat treatment at 600 $^{\circ}\Delta C$, the formation of hydroxyapatite has been confirmed by XRD analyses and the substrate material was found to be oxidized with negligible amount of CaO in the coating. The SEM studies revealed surface morphology. Hydroxyapatite, calcined at 600$^{\circ}\Delta C$, displaying a porous structure arisen from heating of the bulk. But, it is very meaningful in trying to approach morale management plans with an object of dental technicians. It is necessary that dental technicians should make efforts to control themselves.

• 대한치과보철학회지
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• 제44권3호
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• pp.343-355
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• 2006

Statement of problem. The success of osseointegration can be enhanced with an implant that has improved surface characteristics. Anodic oxidation is one of the surface modifying method to achieve osseointegration. Voltage of anodic oxidation can change surface characteristics and cell activity Purpose. This study was performed to evaluate MG63 cell responses such as affinity, proliferation and to compare surface characteristics of anodic oxidized titanium in various voltage. Material and method. The disks for cell culture were fabricated from grade 3 commercially pure titanium,1 m in thickness and 12 mm in diameter. Surfaces of 4 different roughness were prepared. Group 1 had a machined surface, used as control. Group 2 was anodized under 220 V, group 3 was anodized under 300 V and group 4 was anodized under 320 V. The microtopography of specimens was observed by scanning electron microscope (JSM-840A, JEOL, Japan) and atomic force microscope(Autoprobe CP, Park Scientific Instrument, USA). The surface roughness was measured by confocal laser scanning microscope(Pascal, LSM5, Zeiss, Germany). The crystal structure of the titanium surface was analyzed with x-ray diffractometer(D8 advanced, Broker, Germany). MG63 osteoblast-like cells were cultured on these specimens. The cell morpholgy was observed by field emission electron microscope(Hitachi S-4700, Japan). The cell metabolic and proliferative activity was evaluated by MTT assay Results and conclusion. With in limitations of this in vitro study, the following conclusions were drawn. 1. In anodizing titanium surface, we could see pores which did not show in control group. In higher anodizing voltage, pore size was increased. 2. In anodizing titanium surface, we could see anatase. In higher anodizing voltage, thicker oxide layer increased crystallinity(anatase, anatase and rutile mixed). 3. MG63 cells showed more irregular, polarized and polygonal shape and developed more lamellipodi in anodizing group as voltage increased. 4. The activity of cells in MTT assay increased significantly in group 3 and 4 in comparison with group 1 and 2. However, there was no difference between group 3 and 4 at P<0.05. Proliferation of MG63 cells increased significantly in pore size($3-5.5{\mu}m$) of group 3 and 4 in comparison with in pore size($0.2-1{\mu}m$ ) of group 2.

• 대한치과보철학회지
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• 제45권6호
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• pp.795-804
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• 2007

Statement of problem. Nano-scale calcium-phosphate coating on the anodizing titanium surface using ion beam-assisted deposition (IBAD) has been recently introduced to improve the early osseointegration. However, not much is known about their surface characteristics that have influence on tissue-implant interaction. Purpose. This study was aimed to investigate microtopography, surface roughness, surface composition, and wettability of the titanium surface modified by the anodic oxidation and calcium phosphate coating using IBAD. Material and methods. Commercially pure titanium disks were used as substrates. The experiment was composed of four groups. Group MA surfaces represented machined surface. Group AN was anodized surface. Group CaP/AN was anodic oxidized and calcium phosphate coated surfaces. Group SLA surfaces were sandblasted and acid etched surfaces. The prepared titanium discs were examined as follows. The surface morphology of the discs was examined using SEM. The surface roughness was measured by a confocal laser scanning microscope. Phase components were analyzed using thin-film x-ray diffraction. Wettability analyses were performed by contact angle measurement with distilled water, formamide, bromonaphtalene and surface free energy calculation. Results. (1) The four groups showed specific microtopography respectively. Anodized and calcium phosphate coated specimens showed multiple micropores and tiny homogeneously distributed crystalline particles. (2) The order of surface roughness values were, from the lowest to the highest, machined group, anodized group, anodized and calcium phosphate deposited group, and sandblasted and acid etched group. (3) Anodized and calcium phosphate deposited group was found to have titanium and titanium anatase oxides and exhibited calcium phosphorous crystalline structures. (4) Surface wettability was increased in the order of calcium phosphate deposited group, machined group, anodized group, sandblasted and acid etched group. Conclusion. After ion beam-assisted deposition on anodized titanium, the microporous structure remained on the surface and many small calcium phosphorous crystals were formed on the porous surface. Nanoscale calcium phosphorous deposition induced roughness on the microporous surface but hydrophobicity was increased.

• Journal of Periodontal and Implant Science
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• 제48권1호
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• pp.60-68
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• 2018

Purpose: The aim of this study was to evaluate the ability of Porphyromonas gingivalis (P. gingivalis) to induce oxidation of high-density lipoprotein (HDL) and to determine whether the oxidized HDL induced by P. gingivalis exhibited altered antiatherogenic function or became proatherogenic. Methods: P. gingivalis and THP-1 monocytes were cultured, and the extent of HDL oxidation induced by P. gingivalis was evaluated by a thiobarbituric acid-reactive substances (TBARS) assay. To evaluate the altered antiatherogenic and proatherogenic properties of P. gingivalistreated HDL, lipid oxidation was quantified by the TBARS assay, and tumor necrosis factor alpha (TNF-${\alpha}$) levels and the gelatinolytic activity of matrix metalloproteinase (MMP)-9 were also measured. After incubating macrophages with HDL and P. gingivalis, Oil Red O staining was performed to examine foam cells. Results: P. gingivalis induced HDL oxidation. The HDL treated by P. gingivalis did not reduce lipid oxidation and may have enhanced the formation of MMP-9 and TNF-${\alpha}$. P. gingivalistreated macrophages exhibited more lipid aggregates than untreated macrophages. Conclusions: P. gingivalis induced HDL oxidation, impairing the atheroprotective function of HDL and making it proatherogenic by eliciting a proinflammatory response through its interaction with monocytes/macrophages.

• 한국재료학회지
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• 제16권10호
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• pp.606-613
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• 2006

This study was purposed to evaluate the influence of anodically oxidized film on titanium (Ti) onto MG-63 osteoblast-like cell attachment and activity. Only scratch lines created by polishing were seen in ASR and ANO-1 groups. About $1.5{\mu}m$-thick homogeneous oxide film which has pores of about $0.5{\mu}m$ diameter were formed in ANO-12. The crystalline structure of the oxide films formed by anodization in phosphoric acid electrolyte was $TiP_2O_7$. The total protein amounts of ANO-1 and ANO-12 groups showed higher values of maximum protein amount than that of AS-R group. At 3 days of incubation, total protein amount showed higher value in ANO-2 when comparing to that of AS-R (p<0.05). Based on the results of ALPase activity test, the degree of MG-63 cell differentiation for initial mineralization matrix formation was similar. For all the test groups after 1 day of incubation, MG-63 cells grew healthily in mono-layer with dendritic extensions. After incubation for 3 days, the specimen surfaces were covered more densely by cells, and numerous micro filaments were extruding to the extracellular matrix.

• Journal of Periodontal and Implant Science
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• 제42권3호
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• pp.81-87
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• 2012

Purpose: The characteristics of oxidized titanium (Ti) surfaces varied according to treatment conditions such as duration time and temperature. Thermal oxidation can change Ti surface characteristics, which affect many cellular responses such as cell adhesion, proliferation, and differentiation. Thus, this study was conducted to evaluate the surface characteristics and cell response of thermally treated Ti surfaces. Methods: The samples were divided into 4 groups. Control: machined smooth titanium (Ti-S) was untreated. Group I: Ti-S was treated in a furnace at $300^{\circ}C$ for 30 minutes. Group II: Ti-S was treated at $500^{\circ}C$ for 30 minutes. Group III: Ti-S was treated at $750^{\circ}C$ for 30 minutes. A scanning electron microscope, atomic force microscope, and X-ray diffraction were used to assess surface characteristics and chemical composition. The water contact angle and surface energy were measured to assess physical properties. Results: The titanium dioxide ($TiO_2$) thickness increased as the treatment temperature increased. Additional peaks belonging to rutile $TiO_2$ were only found in group III. The contact angle in group III was significantly lower than any of the other groups. The surface energy significantly increased as the treatment temperature increased, especially in group III. In the 3-(4,5-Dimethylthiazol- 2-yl)-2,5-diphenyltetrazolium bromide assay, after 24 hours of incubation, the assessment of cell viability showed that the optical density of the control had a higher tendency than any other group, but there was no significant difference. However, the alkaline phosphatase activity increased as the temperature increased, especially in group III. Conclusions: Consequently, the surface characteristics and biocompatibility increased as the temperature increased. This indicates that surface modification by thermal treatment could be another useful method for medical and dental implants.

• 대한치과보철학회지
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• 제45권1호
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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.