• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2017.05a
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• pp.154-154
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• 2017

Ti-6Al-4V alloys are widely used as metal-lic biomaterials in dentistry and orthopedics due to its excellent biocompatibility and me-chanical properties. However, because of low biological activity, it is difficult to form bone growth directly on the surface of titanium implants. For this reason, surface treatment of plasma electrolytic oxidation(PEO) was used for dental implants. To enhance bioac-tivity on the surface, strontium(Sr) and sili-con(Si) ions can be added to PEO treated sur-face in the electrolyte containing these ions. The presence of Sr in the coating enhances osteoblast activity and differentiation, where-as it inhibits osteoclast production and prolif-eration. And Si has been found to be essen-tial for normal bone, cartilage growth, and development. In this study, electrochemical characteristics of Ca, P, Sr, and Si ions from PEO-treated Ti-6Al-4V alloy surface was re-searched using various experimental instruments. DC power is used and Ti-6Al-4V al-loy was subjected to a voltage of 280 V for 3 minutes in the electrolyte containing 5, 10, 20M% Sr ion and 5M% Si ion. The morphol-ogies of PEO-treated Ti-6Al-4V alloy by electrochemical anodization were examined by field-emission scanning electron micro-scopes (FE-SEM), energy dispersive x-ray spectroscopy (EDS), x-ray diffraction (XRD) and corrosion analysis using AC impedance and potentiodynamic polarization test in 0.9% NaCl solution at similar body tempera-ture using a potentiostat with a scan rate of 1.67mV/s and potential range from -1500mV to + 2000mV.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2018.06a
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• pp.74-74
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• 2018

Ti-6Al-4V alloys have been widely used as orthopedic materials because of their excellent corrosion resistance and mechanical properties. However, it does not bind directly to the bone, so it requires a surface modification. This problem can be solved by nanotube and micropore formation. Plasma electrolytic oxidation (PEO) treatment for micropore, which combines high-voltage spark and electrochemical oxidation, is a new way of forming a ceramic coating on light metals such as titanium and its alloys. This method has excellent reproducibility and can easily control the shape and size of the Ti alloy. In this study, formation of bioactive surface by PEO-treatment after $2^{nd}$ ATO technique of Ti-6Al-4V alloy was invesgated by various instrument. Nanotube oxide surface structure was formed on the surface by anodic oxidation treatment in 0.8 wt.% NaF and 1M $H_3PO_4$ electrolytes. After nanotube formation, nanotube layer was removed by ultrasonic cleaning. PEO-treatment was carried out at 280V for 3 minutes in the electrolytic solution containing the bioactive substance (Mg, Zn, Mn, Sr, and Si). The surface of Ti-6Al-4V alloy was observed by field emission scanning electron microscopy (FE-SEM, S-4800 Hitachi, Japan). An energy dispersive X-ray spectrometer (EDS, Inca program, Oxford, UK) was used to analyze the spectra of physiologically active Si, Mn, Mg, Zn, and Sr ions. The PEO film formed on the Ti-6Al-4V alloy surface was characterized using an X-ray diffractometer (TF-XRD, X'pert Philips, Netherlands). It is confirmed that bioactive ions play an essential role in the normal bone growth and metabolism of the human skeletal tissues.

• Journal of the Korean Ceramic Society
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• v.50 no.2
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• pp.108-115
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• 2013

Oxide coatings were prepared on Al-1050 substrates by an environment-friendly plasma electrolytic oxidation (PEO) process using an electrolytic solution of $Na_2SiO_3$ (8 g/L) and NaOH (3 g/L). The effects of three different duty cycles (20%, 40%, and 60%) and frequencies (50 Hz, 200 Hz, and 800 Hz) on the structure and micro-hardness of the oxide coatings were investigated. XRD analysis revealed that the oxides were mainly composed of ${\alpha}-Al_2O_3$, ${\gamma}-Al_2O_3$, and mullite. The proportion of each crystalline phase depended on various electrical parameters, such as duty cycle and frequency. SEM images indicated that the oxide coatings formed at a 60% duty cycle exhibited relatively coarser surfaces with larger pore sizes and sintering particles. However, the oxides prepared at a 20% duty cycle showed relatively smooth surfaces. The PEO treatment also resulted in a strong adhesion between the oxide coating and the substrate. The oxide coatings were found to improve the micro-hardness with the increase of duty cycle. The structural and physical properties of the oxide coatings were affected by the duty cycles.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2018.06a
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• pp.75-75
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• 2018

Commercially pure titanium (CP-Ti) and Ti-6Al-4V alloys have been widely used in implant materials such as dental and orthopedic implants due to their corrosion resistance, biocompatibility, and good mechanical properties. However, surface modification of titanium and titanium alloys is necessary to improve osseointegration between implant surface and bone. Especially, when titanium oxide nanotubes are formed on the surface of titanium alloy, cell adhesion is greatly improved. In addition, plasma electrolytic oxide (PEO) coatings have a good safety for osseointegration and can easily and quickly form coatings of uniform thickness with various pore sizes. Recently, the effects of bone element such as magnesium, zinc, strontium, silicon, and manganese for bone regeneration are researching in dental implant field. The purpose of this study was researched on the surface morphology of PEO-treated Ti-6Al-4V alloy after anodic titanium oxide treatmentusing various instruments. Ti-6Al-4V ELI disks were used as specimens for nanotube formation and PEO-treatment. The solution for the nanotube formation experiment was 1 M $H_3PO_4$ + 0.8 wt. % NaF electrolyte was used. The applied potential was 30V for 1 hours. The PEO treatment was performed after removing the nanotubes by ultrasonics for 10 minutes. The PEO treatment after removal of the nanotubes was carried out in the $Ca(CH_3)_2{\cdot}H_2O+(CH_3COO)_2Mg{\cdot}4H_2O+Mn(CH_3COO)_2{\cdot}4H_2O+Zn(CH_3CO_2)_2Zn{\cdot}2H_2O+Sr(CH_2COO)_2{\cdot}0.5H_2O+C_3H_7CaO_6P$ and $Na_2SiO_3{\cdot}9H_2O$ electrolytes. And the PEO-treatment time and potential were 3 minutes at 280V. The morphology changes of the coatings on Ti-6Al-4V alloy surface were observed using FE-SEM, EDS, XRD, AFM, and scratch tester. The morphology of PEO-treated surface in 5 ion coating solution after nanotube removal showed formation or nano-sized mesh and micro-sized pores.

• 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.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.11 no.7
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• pp.2451-2458
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• 2010

We prepared sustained release matrix system which contains carvedilol with Compritol 888 ATO used as lipophilic sustained release excipient and hydroxypropyl methyl cellulose (HPMC) or polyethylene oxide (PEO) used as hydrophilic sustained release polymer. Wet granulation compressed method was used for preparing carvedilol sustained release matrix tablets. When carvedilol sustained release matrix tablets were prepared, we evaluated the drug release kinetics which is affected by Compritol 888 ATO ratio, a kind of hydrophilic polymer (HPMC, PEO) and hot melt coating coagglutination (HMCC) process was done. The drug release kinetics was measured for 24 hours in pH 1.2 simulated gastric fluid and pH 6.8 simulated intestinal fluid, using a dissolution tester at $37.5^{\circ}C$ in 50 rpm. Dissolution rate of controlled release matrix tablets of carvedilol was evaluated by paddle method. We confirmed that HMCC process was very effective to controlled release of drugs. The rate of Compritol 888 ATO, as a lipidic material, can control the drug release pattern about the elution rate of 95% and 24 hours delay than that of the normal tablet.

• 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.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.120-120
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• 2016

Ti-6Al-4V alloy have been used for dental implant because of its excellent biocompatibility, corrosion resistance, and mechanical properties. However, the integration of such implant in bone was not in good condition to achieve improved osseointergraiton. For solving this problem, calcium phosphate (CaP) has been applied as coating materials on Ti alloy implants for hard tissue applications because its chemical similarity to the inorganic component of human bone, capability of conducting bone formation and strong affinity to the surrounding bone tissue. Various metallic elements, such as strontium (Sr), magnesium (Mg), zinc (Zn), sodium (Na), silicon (Si), silver (Ag), and yttrium (Y) are known to play an important role in the bone formation and also affect bone mineral characteristics, such as crystallinity, degradation behavior, and mechanical properties. Especially, Zn is essential for the growth of the human and Zn coating has a major impact on the improvement of corrosion resistance. Plasma electrolytic oxidation (PEO) is a promising technology to produce porous and firmly adherent inorganic Zn containing $TiO_2(Zn-TiO_2)$coatings on Ti surface, and the a mount of Zn introduced in to the coatings can be optimized by altering the electrolyte composition. In this study, corrosion behavior of Ti-6Al-4V alloy after plasma electrolytic oxidation in solutions containing Ca, P and Zn were studied by scanning electron microscopy (SEM), AC impedance, and potentiodynamic polarization test. A series of $Zn-TiO_2$ coatings are produced on Ti dental implant using PEO, with the substitution degree, respectively, at 0, 5, 10 and 20%. The potentiodynamic polarization and AC impedance tests for corrosion behaviors were carried out in 0.9% NaCl solution at similar body temperature using a potentiostat with a scan rate of 1.67mV/s and potential range from -1500mV to +2000mV. Also, AC impedance was performed at frequencies ranging from 10MHz to 100kHz for corrosion resistance.

• Proceedings of the Korean Vacuum Society Conference
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• 2011.08a
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• pp.161-161
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• 2011

Titanium (IV) dioxide (TiO2) is one of the most attractive d-block transition metal functional oxides. Many applications of TiO2 such as dye-sensitized solar cells and photocatalyst have been widely investigated. To utilize solar energy efficiently, TiO2 should be well-aligned with a high surface area and promote the charge separation as well as electron transport. Herein, the TiO2 nanotubes were successfully fabricated by a template-directed method. The electrospun PEO(Polyethylene oxide, Molecular weight, 400k)fibers were used as a soft template for coating with titanium dioxide using an atomic layer deposition (ALD) technique. The deposition was conducted onto a template at 50$^{\circ}C$ by using titaniumisopropoxide [Ti(OCH(CH3)2)4; TTIP] as precursors of TiO2. While the as-deposited TiO2 layers onto PEO fibers were completely amorphous with atomic layer deposition, the TiO2 layers after calcination at 500$^{\circ}C$ for 1 h were properly converted into polycrystalline nanostructured hallow TiO2 nanotube. The TiO2 nanotube with high surface area can be easily handled and reclaimed for use in future applications related to solar cell fabrications.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2018.06a
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• pp.63-63
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• 2018

본 연구는 플라즈마 전해 산화 (PEO) 및 RF (Radio Frequency) 스퍼터링을 이용한 2 단계 접근법에 의해 처리 된 MgO / Ni-Cr의 고내식성 이중층 코팅을 제조하기 위해 수행되었다. 이를 위해 $100mA/cm^2$ 교류 조건에서 180 s PEO를 한 후 150W 에서 900s RF 스퍼터링을 수행 하였다. 코팅의 형태는 주사전자현미경(SEM)을 사용하여 관찰되었으며 코팅의 상조성은 X-선 회절(XRD) 및 X-선 광전자 분광법(XPS)을 사용하여 분석하였다. SEM 이미지는 스퍼터링 된 Ni-Cr이 크랙의 대부분과 미세한 미세 공극을 덮어 코팅 결함이 감소함을 보여 주었다. 따라서, 코팅 된 샘플의 거칠기 값은 스퍼터링 공정 후에 감소되었다. 단면 이미지로부터, 스퍼터링된 코팅층은 낮은 두께 때문에 거의 검출되지 않았다. EDS, XRD 및 XPS를 사용한 조성 분석은 금속 상태의 형태로 Ni 및 Cr 존재를 나타내었고 XPS에서 NiCr2O4 부동태 피막이 검출되었다. MgO / Ni-Cr 이중층 코팅의 내부식성은 MgO / Ni-Cr 이중층을 가진 샘플의 금속 원소와 비교하여 우수한 부식 특성을 나타내는 전위 역학적 분극 시험 및 전기 화학적 임피던스 분광법으로 평가 하였다.