• 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.

• Korean Journal of Materials Research
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• v.28 no.4
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• pp.201-207
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• 2018

Infrared(IR) heating has many advantages, such as energy efficiency, reduced heating time, cleanliness, equipment compactness, high drying rate and easy automation. These features of IR heating provide widely industrial applications, such as surface heat treatment in semiconductor fabrication, thermoforming of polymers, drying and disinfection of food products, heating to metal forging, and drying of wet materials. In this study, the characteristics of a protected gold mirror were examined by spectrophotometer and the lifetime of the coating layers were evaluated by a cross-cutting method and salt spray test. The effects of manufacturing conditions on the protected gold mirror were seen and remedies for these effects were noted in order to improve the properties of the protected gold mirror in the drying process. The reflectance and lifetime of the protected gold mirror was influenced by manufacturing conditions, such as surface roughness and forming conditions of the anti-oxide layer, the adhesion layer, the reflecting layer and the protection layer. The results of this study showed that the protected gold mirror manufactured using a buffing method for pre-treatment resulted in the most effective reflectance. In addition, $Al_2O_3$ coating on an Al substrate as an anti-oxide layer was more effective than the anodizing process in the test of reflectance. Furthermore, the protected gold mirror manufactured by layers forming of various materials resulted in the most effective reflectance and lifetime when coated with $Al_2O_3$ as the anti-oxide layer, coated Cr as the adhesion layer, and coated $MgF_2$ as the protection layer.

• 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.

• Korean Journal of Materials Research
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• v.11 no.4
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• pp.329-334
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• 2001

Microstructures of barrier-type oxide layers on aluminum was studied by XRD, TEM and RBS. Fer formation of oxide layer. aluminum was anodized in a boric acid solution. The thickness of the oxide film subjected to applied voltage increased linearly at ratio of 1.54nm/V. For oxide layer anodized at 300V, amorphous structure of oxide layer was not transformed after heat treatment at 50$0^{\circ}C$ , while for oxide layers anodized at higher voltages the amorphous structure crystallized into a ${\gamma}$-alumina without any heat treatment. It was also found that the amorphous structure of oxide layer formed at 100V transformed into crystalline structure by electron irradiation. The structure was identified as ${\gamma}$-alumina.

• 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.

• Korean Journal of Materials Research
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• v.29 no.10
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• pp.609-616
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• 2019

Oxide coatings are formed on die-cast AZ91D Mg alloy through an environmentally friendly plasma electrolytic oxidation(PEO) process using an electrolytic solution of $NaAlO_2$, KOH, and KF. The effects of PEO condition with different duty cycles (10 %, 20 %, and 40 %) and frequencies(500 Hz, 1,000 Hz, and 2,000 Hz) on the crystal phase, composition, microstructure, and micro-hardness properties of the oxide coatings are investigated. The oxide coatings on die-cast AZ91D Mg alloy mainly consist of MgO and $MgAl_2O_4$ phases. The proportion of each crystalline phase depends on various electrical parameters, such as duty cycle and frequency. The surfaces of oxide coatings exhibit as craters of pancake-shaped oxide melting and solidification particles. The pore size and surface roughness of the oxide coating increase considerably with increase in the number of duty cycles, while the densification and thickness of oxide coatings increase progressively. Differences in the growth mechanism may be attributed to differences in oxide growth during PEO treatment that occur because the applied operating voltage is insufficient to reach breakdown voltage at higher frequencies. PEO treatment also results in the oxide coating having strong adhesion properties on the Mg alloy. The micro-hardness at the cross-section of oxide coatings is much higher not only compared to that on the surface but also compared to that of the conventional anodizing oxide coatings. The oxide coatings are found to improve the micro-hardness with the increase in the number of duty cycles, which suggests that various electrical parameters, such as duty cycle and frequency, are among the key factors controlling the structural and physical properties of the oxide coating.

• Journal of the Korean Electrochemical Society
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• v.6 no.2
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• pp.145-152
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• 2003

Capacitance of a hybrid capacitor that has characteristics of both electrolyte capacitor and supercapacitor is determined by anode surface covered with oxide layer. In this study, optimal condition processes for anode to fabricate a high voltage hybrid capacitor was investigated. We mixed aluminum powder having mean particle size of $40{\mu}m$ with NaCl powders at weight ratio of 4 : 1 and prepared a disk type electrode after annealing at various temperature. After dissolving NaCl in $50^{\circ}C$ distilled water, heat treatment, eletropolishing, chemical treatment, and the first and the second etching of Al disk were conducted. In each process, capacitances and resistances of the disk measured by ac-impedance analyzer were compared to find its optimum treatment condition. Also, the surface morphology of treated disks were observed and compared by SEM. After the second etching, the Al disk was anodized at 365V to make an anode of hybrid supercapacitor that can be operated at 300V, Capacitance and resistance of the anodized Al disk electrode was compared with those of commercialized conventional aluminum electrolytic capacitor at different frequencies.

• Journal of Technologic Dentistry
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• v.27 no.1
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• pp.79-88
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• 2005

This study was performed to investigate the surface properties of electrochemically oxidized pure niobium by anodic oxide and hydrothermal treatment technique. Niobium specimens of $10\times10mm$ in dimension were polished sequentially from #600, #800, #1000 emery paper. The surface pure niobium specimens were anodized in an electrolytic solution that was dissolved calcium and phosphate in water. The electrolytic voltage was set in the range of 250 V and the current density was 10 $mA/cm^2$. The specimen was hydrothermal treated in high-pressure steam at 300$^{\circ}C$ for 2 hours using an autoclave. Then, specimens were immersed in the Hanks' solution with pH 7.4 at 37$^{\circ}C$ for 30 days. The surface of specimen was characterized by scanning electron microscope(SEM), energy dispersive X-ray microanalysis(EDX), potentiostat/galvanostat test, and cytotoxicity test. The results obtained was summarized as follows; According to the result of measuring corrosion behavior at 0.9% NaCl, corrosion resistance was improved more specimens treated with anodic oxide than in hydrothermal treated ones. The multi-porous oxide layer on surface treated through anodic oxidation showed a structure that fine pores overlap one another, and the early precipitation of apatite was observed on the surface of hydrothermal treated samples. According to the result of EDX after 30 days deposition in Hanks' solution, Ca/P was 1.69 in hydrothermal treated specimens. In MTT test, specimens treated through anodic oxidation and hydrothermal treated ones showed spectrophotometer similar to that of the control group. Thus no significant difference in cytotoxicity was observed (P>0.05).

• 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%.

• The Journal of Korean Academy of Prosthodontics
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• v.49 no.4
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• pp.333-340
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• 2011

Purpose: The aim of this study was to study the effect of hydroxyapatite (HA) coating crystallinity on the proliferation and differentiation of human osteosarcoma cells. Materials and methods: Surface roughness of the titanium disks increased by anodizing treatment and then HA was coated using ion beam-assisted deposition (IBAD). HA coating was crystallized by heat-treated at different temperature ($100^{\circ}C$, $300^{\circ}C$, $500^{\circ}C$, $800^{\circ}C$). According to the temperature, disks were divided into four groups (HA100, HA300, HA500, HA800). With the temperature, crystallinity of the HA coating was different. Anodized disks were used as control group. The physical properties of the disk surface were evaluated by surface roughness tests, XRD tests and SEM. The effect of the crystallinity of HA coating on HOS cells was studied in proliferation and differentiation. HOS cells were cultured on the disks and evaluated after 1, 3, 5, and 7 days. Growth and differentiation kinetics were subsequently investigated by evaluating cell proliferation and alkaline phosphatase activity. Results: Regardless of the heat-treated temperature, there is no difference on the surface roughness. Crystallinity of the HA was appeared in the groups of HA500, HA800. HOS cells proliferation, ALP activity were higher in HA500 and HA800 group than HA100 and HA300. Conclusion: Within the results of this limited study, heat treatment at $500^{\circ}C$ of HA coating produced by IBAD has shown greater effect on proliferation and differentiation of HOS cells. It is considered that further in vivo study will be necessary.