• The Journal of Korean Academy of Prosthodontics
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• v.45 no.3
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• pp.362-374
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• 2007

Statement of problem. The intial stability for osseointegration of implant has been an interesting factor. Especially, in the case of poor bone quality or immediately loaded implant, various strategies have been developed focusing on the surface of materials to improve implant fixation to bone. The microscopic properties of implant surfaces play a major role in the osseous healing of dental implants. Purpose. The aims of this study are to perform a histologic and histomorphometric comparison of the healing characteristics of three different surfaces and the comparison of resonance frequency analysis (RFA) values measured by $Osstell^{TM}$ and perio-test values (PTV) measured by Periotest. Material and methods. A total of 24 screw titanium implants (Dentium Co., Seoul, Korea) with 6mm in length and 3.4mm in diameter, were placed in the mandible of 4 beagle dogs. Implants were divided into three groups following the surface treatment methods: Group I is machined(control group). Group II is anodically oxidized. Group III is coated 500nm in thickness with hydroxyapatite(HA) by ion beam assisted deposition(IBAD) on the anodized oxidization. Bone blocks from 2 dogs were caught after 3 weeks of covered healing and another blocks from 2 dogs after 6 weeks. RFA values and PTV were measured right after insertion and at 3 and 6weeks. Histomorphometric analysis was made with Kappa Image Base System to calculate bone-to-implant contact (BIC) and bone area inside the threads. Pearson's correlation analyses were performed to evaluate the correlation between RFA and PTV, BIC and bone area ratio of three different surfaces at 3 and 6 weeks. Results. 1) In all surface treatment methods, the RFA values decreased and the PTV values increased until 6 weeks in comparison to initial values. 2) At 3 weeks, no significant difference was found from bone-to-implant contact ratio and bone area ratio of three different surface treatment methods(P>0.05). However, at 6 weeks, different surface treatment methods showed significantly different bone-toimplant contact ratio and bone area ratio(P<0.05). 3) In the implants with the IBAD on the anodic oxidization, significant difference was found between the 3 weeks and the 6 weeks bone area ratio(P<0.05). 4) Correlation was found between the RFA values and the bone area ratio at 3 and 6 weeks with significant difference(P<0.05). Conclusions. These results indicate that the implants with the IBAD on the anodic oxidization may have a high influence on the initial stability of implant.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2017.05a
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• pp.158-158
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• 2017

Titanium and its alloys have been used in the field dental and orthopedic implants because of their excellent mechanical properties and biocompatibility. Despite these attractive properties, their passive films were somewhat bioinert in nature so that sufficient adhesion of bone cells to implant surface was delayed after surgical treatment. Recently, plasma electrolyte oxidation (PEO) of titanium metal has attracted a great deal of attention is a comparatively convenient and effective technique and good adhesion to substrates and it enhances wear and corrosion resistances and produces thick, hard, and strong oxide coatings. Silicon(Si), Zinc(Zn), and Manganese(Mn) have a beneficial effect on bone. Si in particular has been found to be essential for normal bone and cartilage growth and development. And, Zn has been shown to be responsible for variations in body weight, bone length and bone biomechanical properties. Also, Mn influences regulation of bone remodeling because its low content in body is connected with the rise of the concentration of calcium, phosphates and phosphatase out of cells. The objective of this work was research on bone-like apatite morphology on Si-Zn-Mn-hydroxyapatite coating on Ti-6Al-4V alloy by plasma electrolytic oxidation. Anodized alloys were prepared at 280V voltage in the solution containing Si, Zn, and Mn ions. The surface characteristics of PEO treated Ti-6Al-4V alloy were investigated using XRD, FE-SEM, and EDS.

• Journal of Dental Rehabilitation and Applied Science
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• v.21 no.1
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• pp.33-42
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• 2005

This study was performed to investigate the surface properties and in vitro biocompatibility of electrochemically oxidized Ti-6Al-7Nb alloy by anodic spark discharge technique. Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 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. Anodizing was performed using a regulated DC power supply. The applied voltages were given at 240, 280, 320, and 360 V and current density of $30mA/cm^2$. Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. Samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ during 30 days. The results obtained were summarized as follows; 1. The oxide films were porous with pore size of $1{\sim}5{\mu}m$. The size of micropores increased with increasing the spark forming voltage. 2. The main crystal structure of the anodic oxide film was anatase type as analyzed with thin-film X-ray diffractometery. 3. Needle-like hydroxyapatite (HA) crystals were observed on anodic oxide films after hydrothermal treatment at $300^{\circ}C$ for 2 hours. The precipitation of HA crystals was accelerated with increasing the spark forming voltage. 4. The precipitation of the fine asperity-like HA crystals were observed after being immersed in Hanks' solution at $37^{\circ}C$. The precipitation of HA crystals was accelerated with increasing the spark forming voltage and the time of immersion in Hanks' solution. 5. The Ca/P ratio of the precipitated HA layer was equivalent to that of HA crystal as increasing the spark forming voltage and the time of immersion in Hanks' solution.

• Journal of Dental Rehabilitation and Applied Science
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• v.22 no.1
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• pp.101-110
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• 2006

This study was performed to investigate the surface properties and in vitro biocompatibility of electrochemically oxidized Ti-6Al-7Nb alloy by anodic spark discharge technique. Discs of Ti-6Al-7Nb alloy of 20 mm in diameter and 2 mm in thickness were polished sequentially from #300 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. Anodizing was performed using a regulated DC power supply. The applied voltages were given at 240, 280, 320, and 360 V and current density of $30mA/cm^2$. Hydrothermal treatment was conducted by high pressure steam at $300^{\circ}C$ for 2 hours using a autoclave. Samples were soaked in the Hanks' solution with pH 7.4 at $36.5^{\circ}C$ during 30 days. The results obtained were summarized as follows; 1. The oxide films were porous with pore size of $1{\sim}5{\mu}m$. The size of micropores increased with increasing the spark forming voltage. 2. The main crystal structure of the anodic oxide film was anatase type as analyzed with thin-film X-ray diffractometery. 3. Needle-like hydroxyapatie (HA) crystals were observed on anodic oxide films after hydrothermal treatment at $300^{\circ}C$ for 2 hours. The precipitation of HA crystals was accelerated with increasing the spark forming voltage. 4. The precipitation of the fine asperity-like HA crystals were observed after being immersed in Hanks' solution at $37^{\circ}C$. The precipitation of HA crystals was accelerated with increasing the spark forming voltage and the time of immersion in Hanks' solution. 5. The Ca/P ration of the precipitated HA layer was equivalent to that of HA crystal as increasing the spark forming voltage and the time of immersion in Hanks' solution.

• Journal of the Korean institute of surface engineering
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• v.52 no.6
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• pp.298-305
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• 2019

We investigated a correlation between morphology and photoelectrochemical properties of TiO₂ nanotubes fabricated by well-controlled anodization processes. Anodization in an ethylene-glycol-based electrolyte solution accelerated the rapid grow rate of TiO₂ nanotubes, but also cause problems such as delamination at the interface between TiO₂ nanotubes and a Ti substrate, and debris on the top of the nanotube. The applied voltages for the anodization of TiO₂ were adjusted to avoid the interface delamination. The heat treatment and the anodizing time were also controlled to enhance the crystallinity of the as-prepared TiO₂ nanotubes and to increase the surface area with the varied length of the anodized TiO₂ nanotubes. Additionally, a 2-step anodization process was utilized to remove the debris on the tube top. The photoelectrochemical properties of TiO₂ nanotubes prepared with the carefully tailored conditions were investigated. By removing the debris on TiO₂ nanotubes, applied bias photon-to-current efficiency (ABPE) of TiO₂ nanotubes increased up to 0.33%.

• Journal of Korean Dental Science
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• v.2 no.2
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• pp.12-17
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• 2009

Purpose : To determine whether peri-implant crestal bone loss could be affected by systemic disease, primary ISQ value, implantation method (submerged vs. non-submerged), surface treatment, and bone density Materials and methods : Patients who underwent fixture installation from June 24, 2005 to October 23, 2008 at Seoul National University Bundang Hospital were evaluated. A total of 157 patients (male: 52, female: 85) had 346 fixtures installed. Among them, 49 patients had periapical radiographs taken 1 year after prostheses were first set. A total of 97 fixtures were implanted. In particular, 30 fixtures were installed in patients with systemic diseases such as diabetes mellitus, cardiovascular disease, hypertension, and liver disease. The immediate stability of implants was measured with $Osstell^{tm}$. Implant surface treatment was classified into two groups (RBM, Cellnest (Anodized)), and bone density, into four groups (D1~D4). The bone resorption on the mesial and distal areas of fixtures was measured with periapical radiographs using the paralleling technique, and the mean value was calculated. The length determination program in IMPAX (AGFA, Belgium) was used. Results : At least 332 out of 346 (96%) installed GS II implants were successfully osseointegrated 1 year after prostheses were first set. The mean value of the bone resorption of the installed GS II implants was 0.44mm. The minimum value was 0mm, and the maximum value, 2.85mm. There was a statistically significant difference between the implantation methods (submerged, non-submerged) with regard to the amount of alveolar bone loss 1 year after prostheses were first set (p<0.05). Non-submerged implants showed less crestal bone loss. Note, however, that other variables had no correlation with crestal bone loss (p>0.05). Conclusion : There was a statistically significant difference between the 1-stage method and 2-stage method with regard to the amount of alveolar bone loss 1 year after prostheses were first set. Systemic disease, primary ISQ value, surface treatment, and bone density were not associated with alveolar bone loss. Other variables were assumed to have a correlation with alveolar bone loss.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.146-146
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• 2016

최근 국민 소득향상과 더불어, 여가시간 증가에 따라 해양레저에 대한 관심이 크게 높아지고 있으며, 그에 따라 레저용 선박 수요도 증가하고 있다. 기존 국내 소형 선박의 경우 FRP(fiber-reinforced plastic)재료로 선박을 건조해 왔다. 그러나 해양환경 규제 강화로 FRP 선박의 건조가 감소하고 있으며, 친환경 선박에 대한 필요성이 대두되고 있다. 따라서 FRP재료를 대체하는 선박용 재료로 친환경적이고 가벼운 소재인 알루미늄 합금 재료가 선박건조 분야에서 각광을 받고 있다. 특히 5000계열 Al-Mg 합금은 가공성과 용접성이 우수하여 주로 구조용으로 많이 사용되고 있으나 경량화에 따른 빠른 선속이 유체충격을 증가시켜 선체에 캐비테이션 손상을 일으킬 수 있다. Al-Mg 합금의 경우에 부식성이 대단히 큰 해양환경에서 부식과 캐비테이션 침식이 복합적으로 일어나면 손상이 빠르게 증가되는 경향을 나타내어 선박의 수명을 현저히 단축시켜 경제적인 손실을 초래한다. 따라서 본 연구에서는 해수 내에서 Al-Mg 합금의 캐비테이션 저항성을 향상시키기 위해 알루미늄 합금 표면에 내식성 뿐만 아니라 경도 및 내마모성 등의 기계적 특성이 우수한 산화피막을 형성시키는 양극산화 기술을 적용하고, 다양한 봉공처리(sealing)방법에 따른 캐비테이션 특성을 평가하였다. 캐비테이션 실험은 압전(piezoelectric) 효과를 이용한 진동발생 장치를 사용하여 $30{\mu}m$ 진폭으로 일정하게 유지하였으며, 시편과 혼 팁 사이의 간격은 1mm로 하였다. 캐비테이션 실험 후에는 시편을 초음파 세척하여 진공 건조기에서 24시간 이상 건조한 후 정밀저울로 무게를 측정하였으며, 표면 손상 형상을 분석하기 위해 주사전자현미경(SEM)과 3D현미경을 이용하여 관찰하였다.

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

• Proceedings of the Materials Research Society of Korea Conference
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• 2011.05a
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• pp.241.1-241.1
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• 2011

Numerous possible applications for $ZrO_2$ nanotubes exist such as for catalyst support structures, for sensing or for applications as a solid state electrolyte. Especially, because of a large specific surface area, high efficiency for solid oxide fuel cell (SOFC) application at low temperature can be expected for nanotublar structures in even small size. A zirconium precursor, Tetrakis (ethylmethylamino) zirconium, TEMAZr and $H_2O$ oxidant were used to deposit$ZrO_2$ thin films on an anodized aluminum oxide (AAO) templates having sub-100nm cylindrical pores by atomic layer deposition (ALD) in the temperature range of 150~250$^{\circ}C$. The crystalline structures of as-prepared and post-annealed $ZrO_2$ nanotubes were characterized by x-ray diffraction and high-resolution transmission electron microscopy. The as-prepared samples at $150^{\circ}C$ and $200^{\circ}C$ were showed amorphous, whereas a mixed phase of tetragonal, monoclinic and amorphous polymorph was observed at $250^{\circ}C$. In the bulk, zirconia remains monoclinic phase up to $1,175^{\circ}C$, however, $ZrO_2$ nanotubes were showed tetragonal phase upon post thermal treatments merely at $400^{\circ}C$. This trend may be indicative of high-curvature surfaces of nanotubes and thereby the presence of intrinsic compressive strain. The amount of amorphous structures in the mixed phase as well as as-grown $ZrO_2$ nanotubes were also gradually decreased by subsequent heat treatment.

• Journal of Korean Society of Water and Wastewater
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• v.29 no.1
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• pp.33-38
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• 2015

In this study, flat-type photocatalytic reaction system is applied to reduce toxic hexavalent chromium (Cr(VI)) to trivalent chromium (Cr(III)) in aqueous solution under UV irradiation. To overcome the limitation of conventional photocatalysis, a novel approach toward photocatalytic system for reduction of hexavalent chromium including nanotubular $TiO_2$ (NTT) on two kinds of titanium substrates (foil and mesh) were established. In addition, modified Ti substrates were prepared by bending treatment to increase reaction efficiency of Cr(VI) in the flat-type photocatalytic reactor. For the fabrication of NTT on Ti substrates, Ti foil and mesh was anodized with mixed electrolytes ($NH_4F-H_2O-C_2H_6O_2$) and then annealed in ambient oxygen. The prepared NTT arrays were uniformly grown on two Ti substrates and surface property measurements were performed through SEM and XRD. Hydraulic retention time(HRT) and substrate type were significantly affected the Cr(VI) reduction. Hence, the photocatalytic Cr(VI) reduction was observed to be highest up to 95% at bended(modified) Ti mesh and lowest HRT. Especially, Ti mesh was more effective as NTT substrate in this research.