• The Journal of Korean Academy of Prosthodontics
• /
• v.47 no.1
• /
• pp.39-45
• /
• 2009

Statement of problem: Recently precalcification treatment has been studied to shorten the period of the implant. Purpose: This study was performed to evaluate the effect of precalcification treatment of $TiO_2$ Nanotube formed on Ti-6Al-4V Alloy. Material and methods: Specimens of $20{\times}10{\times}2\;mm$ in dimensions were polished sequentially from #220 to #1000 SiC paper, ultrasonically washed with acetone and distilled water for 5 min, and dried in an oven at $50^{\circ}C$ for 24 hours. The nanotubular layer was processed by electrochemical anodic oxidation in electrolytes containing 0.5 M $Na_2SO_4$ and 1.0 wt% NaF. Anodization was carried out using a regulated DC power supply (Kwangduck FA, Korea) at a potential of 20 V and current density of $30\;㎃/cm_2$ for 2 hours. Specimens were heat-treated at $600^{\circ}C$ for 2 hours to crystallize the amorphous $TiO_2$ nanotubes, and precalcified by soaking in $Na_2HPO_4$ solution for 24 hours and then in saturated $Ca(OH)_2$ solution for 5 hours. To evaluate the bioactivity of the precalcified $TiO_2$ nanotube layer, hydroxyapatite formation was investigated in a Hanks' balanced salts solution with pH 7.4 at $36.5^{\circ}C$ for 2 weeks. Results: Vertically oriented amorphous $TiO_2$ nanotubes of diameters 48.0 - 65.0 ㎚ were fabricated by anodizing treatment at 20 V for 2 hours in an 0.5 M $Na_2SO_4$ and 1.0 NaF solution. $TiO_2$ nanotubes were composed with strong anatase peak with presence of rutile peak after heat treatment at $600^{\circ}C$. The surface reactivity of $TiO_2$ nanotubes in SBF solution was enhanced by precalcification treatment in 0.5 M $Na_2HPO_4$ solution for 24 hours and then in saturated $Ca(OH)_2$ solution for 5 hours. The immersion in Hank's solution for 2 weeks showed that the intensity of $TiO_2$ rutile peak increased but the surface reactivity decreased by heat treatment at $600^{\circ}C$. Conclusion: This study shows that the precalcified treatment of $TiO_2$ Nanotube formed on Ti-6Al-4V Alloy enhances the surface reactivity.

• The Journal of Korean Academy of Prosthodontics
• /
• v.49 no.3
• /
• pp.245-253
• /
• 2011

Purpose: The aim of this in vitro study was to estimate surface characteristic after peptide coating and investigate biological response of human mesenchymal stem cell to anodized titanium discs coated with RGD peptide by physical adhesion and chemical fixation. Materials and methods: Fluorescence isothiocyanate (FITC) modified RGD-peptide was coated on the anodized titanium discs (diameter 12 mm, height 3 mm) using two methods. One was physical adhesion method and the other was chemical fixation method. Physical adhesion was performed by dip and dry procedure, chemical fixation was performed by covalent bond via silanization. In this study, human mesenchymal stem cell was used for experiments. The experiments consisted of surface characteristic evaluation after peptide coating, analysis about cell adhesion, proliferation, differentiation, and mineralization. Obtained data are statistically treated using Kruskal-Wallis test and Bonferroni test was performed as post hoc test (P=.05). Results: The evaluation of FE-SEM images revealed no diffenrence at micro-surfaces between each groups. Total coating dose was higher at physical adhesion experimental group than at chemical fixation experimental group. In cell adhesion and proliferation, RGD peptide coating did not show a statistical significance compared with control group (P>.05). In cell differentiation and mineralization, physical adhesion method displayed significantly increased levels compared with control group and chemical fixation method (P<.05). Conclusion: RGD peptide coating seems to enhance osseointegration by effects on the response of human mesenchymal stem cell. Especially physical adhesion method showed more effective than chemical fixation method on response of human mesenchymal stem cell.

• The Journal of Korean Academy of Prosthodontics
• /
• v.53 no.1
• /
• pp.9-18
• /
• 2015

Purpose: The purpose of this study is to examine characteristics of implant surface with RBM and anodizing treatments, and to evaluate the responses of osteoblast-like cell (MG-63 cell). Materials and methods: Grade IV titanium disks were fabricated (Diameter 10 mm, thickness 3 mm). Anodizing treatment (ASD) group, RBM and anodizing treatment (RBM/ASD) group, control (machined surface) group were divided. In this study, osteoblast-like cell was used for experiments. The experiments consist of surface characteristics evaluation by FE-SEM images, energy dispersive spectroscopy and stereo-SEM. In order to evaluate cell adhesion evaluation by crystal violet assay and observe cells form by confocal laser microscopy. To assess cell proliferation by XTT assay, cell differentiation by RT-PCR and mineralization by Alizarin red S stain assay. ELISA analyzer was used for Quantitative evaluation. Comparative analysis was run by one-way ANOVA (SPSS version 18.0). Differences were considered statistically significant at P<.05. Results: In ASD group and RBM/ASD group, the surface shape of the crater was observed and components of oxygen and phosphate ions in comparison with the control group were detected. The surface average roughness was obtained $0.08{\pm}0.04{\mu}m$ in the control group, $0.52{\pm}0.14{\mu}m$ in ASD group and $1.45{\pm}0.25{\mu}m$ in RBM/ASD group. In cell response experiments, ASD group and RBM/ASD group were significantly higher values than control group in cell adhesion and mineralization phase, control group was the highest values in the proliferative phase. In RT-PCR experiments, RBM/ASD group was showed higher ALP activity than other groups. RBM/ASD group in comparison with ASD group was significantly higher value for cell adhesion and proliferation phase. Conclusion: In the limitation of this study, we are concluded that the surface treatment with RBM/ASD seems more effective than ASD alone or machined surface on cellular response.

• Journal of Dental Rehabilitation and Applied Science
• /
• v.24 no.4
• /
• pp.361-369
• /
• 2008

The purpose of this study is to make porous oxide film on the surfaces of pure Ti through anodic spark discharge in electrolytic solution containing calcium and phosphate ions, to improve osseointergration by treating fluoride agent. In addition, it is to evaluate the fluoride modified effect on the surface. Commercial pure Ti plate with $20{\times}10{\times}2mm$ and Ti wire with a diameter of 1.5mm and a total length of 15mm were used. After making titanium oxide films converted by anodic spark discharge, anodizing was performed. Fluoride was spreaded to titanium laboratory plate and maintained for 30 minutes after anodizing breakdown. Fluoride ion discharge amount was measured per 24 hours after dipping titanium plate into saline (10ml) and sustaining 90rpm in a pyrostat. Some plates and wires were dipped in Hanks solutions for a month to examine biocompatibility using SEM and XRD. $TiO_2$ film formed by anodic discharge technique showed great roughness and uniform pores which were $1{\sim}3{\mu}m$ in a diameter. Roughness of the films treated with anodic discharge after blasting were higher than the turned ones(P<0.05). Rapid surface activity was observed in the samples treated with $TiF_3$ agent, which immersed in Hanks solution for 30 days. Taking the results into consideration, the fluoride modified implant with anodic discharge demonstrates that it makes uniformly porous oxide film on the surface of implant and properly increase roughness for osseointegration. The implants will achieve greater bone integration after short healing time by improving surface activity.

• The Journal of Korean Academy of Prosthodontics
• /
• v.50 no.1
• /
• pp.44-52
• /
• 2012

Purpose: In this paper we tried to evaluate the most appropriate surface for rhBMP-2 coating among 4 rough titanium surfaces. Materials and methods: We used machined surface as a control group and anodized, RBM and SLA surfaces as test groups. We coated rhBMP-2 on the 4 surfaces and with uncoated surfaces for each case, we cultured human mesenchymal stem cells on all 8 surfaces. 24 hours after we measured the stem cell' attachment with SEM, and on 3rd, 7th, and 14th days, we checked the cell proliferation and differentiation by using MTT and ALP activity assay. And on the 7th day after the culture, we performed RT-PCR assay to determine whether the expression levels of Type I collagen, osteocalcin, osteopontin were changed. Results: We observed with SEM that 4 rhBMP-2 coated surfaces exhibited wider and tighter cell attachment and more cell process spreading than uncoated surfaces. The anodized rhBMP-2 surface caused robustest effects. In MTT assay we could not find any meaningful difference. In ALP assay there was a significant increase (P<.05) in the ALP activity of anodized rhBMP-2 coated surface compared with that of the control (3rd and 14th days) and with that of the RBM rhBMP-2 coated surface (14th day). In RT-PCR assay there was increased expressions in the anodized rhBMP-2 coated surface for osteocalcin, and osteopontin. Conclusion: We found that the anodized rhBMP-2 coated surface were most prominent stem cell attachment and differentiation in compared to control and Machined rhBMP-2 coated, RBM rhBMP-2 coated surface.

• Journal of Life Science
• /
• v.16 no.2 s.75
• /
• pp.302-309
• /
• 2006

To evaluate the biocompatibility of untreated and anodized titanium specimens, the specimens were implanted in the subcutaneous tissue of the abdominal region of female mice for two weeks. The reaction of connective tissue to specimens was histologically studied. The implants were encapsulated by fibrous connective. tissue consisting of fibroblast, fibrocyte and other cellss including neutroophil, macrophage and giant multinucleated cell. some newly formed blood vessels were located in the fibrous capsule surrounding the implant. Giant multinucleated cells were observed at the fibrous capsule adjacent to the implant. Kind of cell types and the thickness of fibrous capsules were examined quantitatively. Most of cell types located in the fibrous capsule were fibroblast and fibrocyte. The average thickness of fibrous capsules for the anodized specimens was much thinner than that of the untreated titanium specimen. Biocompatibility of titanium specimens were also studied by using cell culture method. The number of MG-63 cells was significantly increased on the anodized titanium specimens in vitro experiment. Our observations suggest that anodized titanium specimens are more effective for the improvement of biocompatibility in vivo and in vitro.

• Journal of dental hygiene science
• /
• v.11 no.5
• /
• pp.405-410
• /
• 2011

The aim of this study was to evaluate antibacterial effect of Cl coated titanium. To coat the Cl on the titanium, first, the titanium was modified by blasting treatment with hydroxyapatite and alumina powder. Anodization process was completed using electrolyte solution of 0.04 M ${\beta}$-glycerol phosphate disodium salt n-hydrate, 0.4 M calcium acetate n-hydrate and 1 M NaCl on the condition of 250 voltages for 3 min. Surface morphology and elements' observation were performed with scanning electron microscopy and energy dispersive spectroscopy and surface profiler was used to analyze the surface roughness. Antibacterial effect was evaluated by film adhesion method. The anodized titanium after blasting showed dimpled surface contained the Cl. Surface average roughness of these surfaces had significantly higher compared to polished titanium. Result of antibacterial test showed that anodized titanium after blasting had an enhanced antibacterial effect compared to the polished titanium. Therefore, these results suggested that titanium contained Cl by anodization after blasting had a rough surface as well as antibacterial effect.

• Journal of Dental Rehabilitation and Applied Science
• /
• v.25 no.1
• /
• pp.41-52
• /
• 2009

The surface treatment of titanium implant could bring out the biochemical bonding between bone and implant. The purpose of this study was to evaluate the biomechanical bone response of Mg-ion implanted implants with plasma source ion implantation method. Twelve New Zealand white rabbits were included in this study. Each rabbit received one control fixture (blasted with resorbable blasting media, RBM) and three types of Mg ion implanted fixtures in tibiae. The implants were left in place for 6 weeks before the rabbits were sacrificed. Removal torque value and resonance frequency analysis (ISQ) were compared. The repeated measured analysis of variance was used with $P{\leq}0.05$ as level of statistical significance. ISQ was not different among all groups. However, the ISQ was increased after 6 weeks healing. The group had lowest ISQ value showed the greatest increment. Mg-1 implants with 9.4% retained ion dose showed significantly higher removal torque value than that of the other implants. From this results, it is concluded that the Mg-1 implants has stronger bone response than control RBM surface implant.

• The Journal of Korean Academy of Prosthodontics
• /
• v.52 no.1
• /
• pp.9-17
• /
• 2014

Purpose: The purpose of this study was to compare zirconia implants with titanium implants from the view point of biomechanical stability and histologic response on osseointegration when those were placed with xenograft materials. Materials and methods: Specimens were divided into two groups; the control group was experimented with eighteen titanium implants which had anodized surface and the experimental group was experimented with eighteen sandblasted zirconia (Y-TZP) implants. At the tibias of six pigs, implants were installed into bone defect sites prepared surgically and treated with resorbable membranes and bovine bone. Two pigs were sacrificed after 1, 4 and 12 weeks respectively. Each implant site was sampled and processed for histologic and histomorphometric analysis. The stability of implants was evaluated with a $Periotest^{(R)}$. And the interfaces between bone and the implant were observed with a scanning electron microscope. Results: In stability analysis there was no significant difference between Periotest values of the control group and the experimental group. In histologic analysis with a light microscope after 4 weeks, there was new bone formation with the resorption of bovine bone and the active synthesis of osteoblasts in both groups. In bone-implant contact percentage there was significant difference between both groups (P<.05). In bone area percentage there was no significant difference between both groups. In analysis of both groups with a scanning electron microscope there was a gap between bone and a surface at 4 weeks and it was filled up with bone formed newly at 12 weeks. Conclusion: When accompanied by xenograft using membrane, bone to implant contact percentage of zirconia implants used in this experiment was significantly less than that of the titanium implants by surface treatment of anodic oxidation. So, it is considered that the improvement of zirconia implant is needed through ongoing research on surface treatment methods for its practical use.

• Journal of Periodontal and Implant Science
• /
• v.35 no.4
• /
• pp.891-905
• /
• 2005

The present study was performed to evaluate the effect of tetracycline-HCL on the change of implant surface microstructure according to application time. Implant with pure titanium machined surface. HA-coated surface and TiUniteTM surface were utilized. Implant surface was rubbed with 50mg/ml tetracycline-HCL solution for $\frac{1}{2}min.$, 1min., $1\frac{1}{2}min.$, 2min., and $2\frac{1}{2}min.$ respectively in the test group. Then, specimens were processed for scanning electron microscopic observation. The results of this study were as follows. 1. Both test and control group showed a few shallow grooves and ridges in pure titanium machined surface implants. There were not significant differences between two groups. 2. In HA-coated surfaces, round particles were deposited irregularly. The roughness of surfaces conditioned with tetracycline-HCL was lessened and the cracks were increased relative to the application time. 3. The anodic oxidized surfaces showed the craterous structures. The surface conditioning with tetracycline-HCl didn't influence on its micro-morphology. In conclusion, the detoxification with 50mg/ml tetracycline-HCL must be applied respectively with different time according to various implant surfaces.