• Journal of the Korean institute of surface engineering
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• v.51 no.1
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• pp.1-10
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• 2018

Anodic oxidation treatment of metals is one of typical surface finishing methods which has been used for improving surface appearance, bioactivity, adhesion with paints and the resistances to corrosion and/or abrasion. This article provides fundamental principle, type and characteristics of the anodic oxidation treatment methods, including anodizing method and plasma electrolytic oxidation (PEO) method. The anodic oxidation can form thick oxide films on the metal surface by electrochemical reactions under the application of electric current and voltage between the working electrode and auxiliary electrode. The anodic oxide films are classified into two types of barrier type and porous type. The porous anodic oxide films include a porous anodizing film containing regular pores, nanotubes and PEO films containing irregular pores with different sizes and shapes. Thickness and defect density of the anodic oxide films are important factors which affect the corrosion resistance of metals. The anodic oxide film thickness is limited by how fast ions can migrate through the anodic oxide film. Defect density in the anodic oxide film is dependent upon alloying elements and second-phase particles in the alloys. In this article, the principle and mechanisms of formation and growth of anodic oxide films on metals are described.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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• pp.217-217
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• 2012

플라즈마 전해산화(Plasma Electrolytic Oxidation)는 수용액 중에서 Al, Mg, Ti 등의 금속표면에 산화막을 형성시키는 기술로서, 기존의 양극산화법과 유사한 장치에서 고전압을 가해 미세플라즈마 방전을 유도하여 치밀한 산화막을 형성하는 표면처리 기술이다. 본 연구에서는 6061 알루미늄 합금의 대면적 시편을 이용하여 PEO공정으로 산화막을 형성시켰다. 산화막의 조성 및 미세구조는 XRD와 SEM, EDS를 이용하여 분석하였다. 형성된 산화막은 회색에서 밝은 회색으로 시편 전면에 고르게 나타났다. 피막 성장인자를 정교하게 조절함으로써 강한 피막 접착력과 낮은 표면조도를 가지는 매끈한 표면을 얻을 수 있었고, 그에 따른 물성 변화를 분석하였다. 또한 시편의 크기에 관계없이 동일한 조건에서 동일한 물성이 나오는 것으로 분석되었다. 이를 통해 균질한 대면적 피막의 높은 신뢰성을 요구하는 다양한 산업분야에 적합한 표면처리 방법으로서 PEO공정이 활용될 수 있음을 확인하였다.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2018.06a
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• pp.70.2-70.2
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• 2018

플라즈마 전해 산화(Plasma Electrolytic Oxidation)는 일반 애노다이징 보다 더 높은 전류 혹은 전압을 금속(Al, Ti, Mg) 표면에 인가하여 산화피막을 전기화학적으로 형성시키는 금속표면처리 방법 중의 하나이다. 본 연구에서는 phosphate 수용액에서 정전류를 인가하여 NaOH의 농도에 따라 PEO(Plasma Electrolytic Oxidation) 피막 형성을 전압-시간 그래프 및 형성된 표면피막의 구조를 관찰하여 연구하였다. 실험에는 8 g/L의 sodium phosphate이 사용되었으며, 5 g/L ~ 9 g/L의 NaOH를 사용하였다. NaOH의 농도 상관없이 일부 영역에서만 반복적으로 아크가 발생하는 로컬 버닝 현상 없이 미세한 아크가 시표 표면 전체에 발생하였고, NaOH의 농도가 증가할수록 형성된 PEO 피막의 두께는 감소하고, 평균 표면 거칠기는 증가하는 경향을 보인다. 형성된 피막의 구조를 HR-SEM, EDX 등을 이용하여 관찰하였다.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2018.06a
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• pp.29.2-29.2
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• 2018

플라즈마 전해 산화(Plasma Electrolytic Oxidation)는 일반 애노다이징 보다 더 높은 전류 혹은 전압을 금속(Al, Ti, Mg) 표면에 인가하여 산화피막을 전기화학적으로 형성시키는 금속표면처리 방법 중의 하나이다. 본 연구에서는 phosphate 수용액에서 정전류를 인가하여 NaOH의 농도에 따라 PEO(Plasma Electrolytic Oxidation) 피막 형성을 전압-시간 그래프 및 형성된 표면피막의 구조를 관찰하여 연구하였다. 실험에는 8 g/L의 sodium phosphate이 사용되었으며, 5 g/L ~ 9 g/L의 NaOH를 사용하였다. NaOH의 농도 상관없이 일부 영역에서만 반복적으로 아크가 발생하는 로컬 버닝 현상 없이 미세한 아크가 시표 표면 전체에 발생하였고, NaOH의 농도가 증가할수록 형성된 PEO 피막의 두께는 감소하고, 평균 표면 거칠기는 증가하는 경향을 보인다. 형성된 피막의 구조를 HR-SEM, EDX 등을 이용하여 관찰하였다.

• Corrosion Science and Technology
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• v.17 no.3
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• pp.91-100
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• 2018

Development of biodegradable implants for treatment of complex bone fractures has recently become one of the priority areas in biomedical materials research. Multifunctional corrosion resistant and bioactive coatings containing hydroxyapatite $Ca_{10}(PO_4)_6(OH)_2$ and magnesium oxide MgO were obtained on Mg-Mn-Ce magnesium alloy by plasma electrolytic oxidation. The phase and elemental composition, morphology, and anticorrosion properties of the coatings were investigated by scanning electron microscopy, energy dispersive spectroscopy, potentiodynamic polarization, and electrochemical impedance spectroscopy. The PEO-layers were post-treated using superdispersed polytetrafluoroethylene powder. The duplex treatment considerably reduced the corrosion rate (>4 orders of magnitude) of the magnesium alloy. The use of composite coatings in inducing bioactivity and controlling the corrosion degradation of resorbable Mg implants are considered promising. We also applied the plasma electrolytic oxidation method for the formation of the composite bioinert coatings on the titanium nickelide surface in order to improve its electrochemical properties and to change the morphological structure. It was shown that formed coatings significantly reduced the quantity of nickel ions released into the organism.

• Journal of the Korean institute of surface engineering
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• v.52 no.5
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• pp.265-274
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• 2019

Formation behavior of PEO (Plasma Electrolytic Oxidation) films on AZ31 Mg alloy was investigated under application of 310 Hz AC as a function of $Na_3PO_4$ concentration from 0.02 M to 0.2 M. Film formation voltage and in-situ observation of arcs generated on the specimen surface were recorded with time, and surface morphologies of the PEO films were investigated using optical microscopy, confocal scanning laser microscopy and scanning electron microscopy. PEO film formation voltage decreased linearly with increasing $Na_3PO_4$ concentration which is attributed to the increase of solution pH. PEO films were grown uniformly over the entire surface in $Na_3PO_4$ solutions between 0.05 M and 0.1 M. However, non-uniform PEO films with white spots were formed in $Na_3PO_4$ solutions containing more than 0.1 M. Thickness and roughness of PEO films on AZ31 Mg alloy increased linearly with increasing $Na_3PO_4$ concentration and their increasing rates appeared to be much higher under 1 M than above 1 M. The experimental results suggest that phosphate ions can contribute to the formation of PEO films but higher $Na_3PO_4$ concentration more than 1 M results in local damages of PEO films due to repeated generation of white arcs at the same surface site of AZ31 Mg alloy.

• Korean Journal of Materials Research
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• v.32 no.6
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• pp.301-306
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• 2022

This study explored the possibility of forming a coating layer containing alginic acid on the surface of a magnesium alloy to be used as a biomaterial. We formed a coating layer on the surface of a magnesium alloy using a plasma electrolytic oxidation process in an electrolytic solution with different amounts of alginic acid (0 g/L ~ 8 g/L). The surface morphology of all samples was observed, and craters and nodules typical of the PEO process were formed. The cross-sectional shape of the samples confirmed that the thickness of the coating layer became thicker as the alginic acid concentration increased. It was confirmed that the thickness and hardness of the sample significantly increase with increasing alginic acid concentration. The porosity of the surface and cross section tended to decrease as the alginic acid concentration increased. The XRD patterns of all samples revealed the formation of MgO, Mg₂SiO₄, and MgF₂ complex phases. Polarization tests were conducted in a Stimulate Body Fluid solution similar to the body's plasma. We found that a high amount of alginic acid concentration in the electrolyte improved the degree of corrosion resistance of the coating layer.

• Journal of the Korean institute of surface engineering
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• v.50 no.6
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• pp.439-446
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• 2017

Plasma electrolyte oxidation (PEO) is a kind of anodization, in which a very high voltage or current is applied to a metal substrate in various electrolytes, allowing distinctly thick thickness of the oxide film with outstanding film properties, such as a good corrosion resistance, mechanical strength, thermal stability, and excellent adhesion to a substrate. Herein, we tried to find the optimal pretreatment conditions among commercially available solutions in order to produce PEO anodizing at relatively low voltage. We characterized the surface morphologies of the sample by scanning electron microscope (SEM), atomic force microscopy (AFM), and investigated color parameters of the pretreated surface of Ti by spectrophotometer.

• Journal of the Korean institute of surface engineering
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• v.49 no.1
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• pp.46-53
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• 2016

The structure of plasma electrolytic oxidation (PEO) coatings was investigated as a function of NaOH concentration in 0.06 M $Na_2SiO_3$ + 0.06 M $Na_3PO_4$ solution by using SEM and epoxy replica method. The PEO film was formed on AZ31 Mg alloy by the application of anodic pulse current with 0.2 ms width and its formation behavior was studied by voltage-time curves during the formation of PEO films. It was found that the addition of NaOH into $PO_4{^{3-}}$ and $SiO_3{^{2-}}$ containing aqueous solution causes a decrease in the PEO film formation voltage, suggesting that dielectric breakdown of the PEO becomes easier with increasing $OH^-$ ion concentration in the solution. With increasing $OH^-$ ion concentration, thickness of the PEO film increased and surface roughness decreased. The size of pores formed in the PEO layer became smaller and the number of cracks in the PEO layer increased with increasing $OH^-$ ion concentration. Based on the experimental results obtained in the work, it is suggested that $OH^-$ ions in the solution can contribute not only to the dielectric breakdown but also to the formation of PEO films in the presence of $PO_4{^{3-}}$ and $SiO_3{^{2-}}$ ions in the solution.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2017.05a
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• pp.98.1-98.1
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• 2017

본 연구에서는 정전류 조건에서 알루미늄 합금의 PEO(Plasma Electrolytic Oxidation) 피막 형성 거동에 대한 전해질 조성의 영향을 아크 발생 양상, 전압-시간 곡선 및 형성된 표면피막의 구조를 관찰하여 연구하였다. 실험에 사용된 전해질은 NaOH 수용액에 $Na_2SiO_3$을 혼합하여 구성되었으며, NaOH와 $Na_2SiO_3$의 농도는 각각 0.01 ~ 1.0 M 와 0 ~ 2.0 M 사이로 조절되었다. 0.01 M NaOH 이하의 용액에서는 양극전압이 500 V 이상으로 상승되고 미세한 아크가 시편 표면 전체에 발생했으나, 0.02 M NaOH 이상의 농도에서는 양극전압이 300 V 이하로 감소되었고 아크발생이 관찰되지 않았다. 아크발생이 일어나지 않는 고농도의 0.5 M NaOH 용액의 경우 0.1 M 이상의 $Na_2SiO_3$를 첨가하였을 때 작은 아크의 무리가 발생되었다. 0.5 M NaOH 수용액에 0.1 M ~ 0.2 M $Na_2SiO_3$가 첨가되었을 땐 아크 무리가 발생하나 이내 일부 영역에서만 반복적으로 아크가 발생하는 로컬 버닝 현상이 일어났다. 한편 0.5 M NaOH 수용액에 0.5 M 이상의 $Na_2SiO_3$가 첨가되었을 때는 로컬 버닝이 일어나지 않고 전 표면에 걸쳐서 아크 무리가 이동하며 PEO 피막이 형성되었다. 0.01 M NaOH 수용액에서 형성된 PEO 피막의 두께는 처리 시간에 따라 증가하지 않고 $10{\mu}m$ 이하의 낮은 값을 보였다. 반면에 NaOH와 $Na_2SiO_3$ 혼합수용액에서 형성된 피막의 두께는 약 $30{\mu}m$ 이상의 높은 값을 보였다.