• 한국융합학회논문지
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• 제7권5호
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• pp.169-173
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• 2016

알루미늄의 양극산화는 황산법, 수산법과 황산과 수산을 활용한 혼산법 등이 있다. 산업체에서 만들어지는 양극산화는 황산법으로 전해액속의 황산농도가 15~20 wt %이다. 연질 양극산화피막을 생성할 경우는 전해액의 온도가 $20{\sim}30^{\circ}C$ 범위에서 생산되고 있으며, 생산 전압은 직류전압으로 13~15 V 이내가 가장 많이 사용된다. 경질 양극산화피막을 생성할 경우는 전해액의 온도가 $0{\sim}-5^{\circ}C$에서 생산되어지고 있다. 본 연구에서는 황산법과 수산법을 이용하여 $50{\mu}m$ 두께의 양극산화피막(알루미나)를 제작하였다. 황산법과 수산법에 의해 시편을 제조하여 열 피로시험을 수행하였다. 황산법과 수산법의 균열발생온도는 $500^{\circ}C$와 $600^{\circ}C$이었다. 황산법의 균열발생온도는 수산법의 균열발생온도보다 낮았다. 시험결과 수산법의 열 피로는 황산법의 열 피로 특성보다 좋았다. 그 이유를 알루미늄과 알루미나의 열팽창계수와 제조온도로 설명하였다. 고온에서 사용되는 양극산화제품의 제조방법을 여기서의 융합 연구를 통해 제안 가능하게 되었다.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2018년도 춘계학술대회 논문집
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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.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2017년도 춘계학술대회 논문집
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• pp.156-156
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• 2017

In this work, analysis of biocompatible TiO2 oxide multilayer by the XPS depth profiling was researched. the manufacture of the TiO2 barrier-type multilayer was accurately performed in a mixed electrolyte containing HAp, Pd, and Ag nanoparticles. The temperature of the solution was kept at approximatively $32^{\circ}C$ and was regularly rotated by a magnetic stirring rod in order to increase the ionic diffusion rate. The manufactured specimens were carefully analyzed by XPS depth profile to investigate the result of chemical bonding behaviors. From the analysis of chemical states of the TiO2 oxide multilayer using XPS, the peaks are showed with the typical signal of Ti oxide at 459.1 eV and 464.8 eV, due to Ti 2p(3/2) and Ti 2p(1/2), respectively. The Pd-3d peak was split into Pd-3d(5/2) and Pd-3d(3/2)peaks, and shows two bands at 334.7 and 339.9 eV for Pd-3d3 and Pd-3d5, respectively. Also, the peaks of Ag-3d have been investigated. The chemical states consisted of the O-1s, P-2p, and Ti-2p were identified in the forms of PO42- and PO43-. Based on the results of the chemical states, the chemical elements into the TiO2 oxide multilayer were also inferred to be penetrated from the electrolyte during anodic process.The structure characterization of the modified surface were performed by using FE-SEM, and from the result of biological evaluation in simulated body fluid(SBF), the biocompatibility of TiO2 oxide multilayer was effective for bioactive property.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2017년도 춘계학술대회 논문집
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• pp.96.2-96.2
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• 2017

This research was conducted to investigate the electrochemical properties of the thin air-formed oxide film-covered AZ31 Mg alloy. In this work, native air-formed oxide films on AZ31 Mg alloy samples were prepared by knife-abrading method and the changes in the electrochemical properties of the air-formed oxide film were investigated in seven different electrolytes containing the following anions $Cl^-$, $F^-$, $SO{_4}^{2-}$, $NO_3{^-}$, $CH_3COO^-$, $CO{_3}^{2-}$ and $PO{_4}^{3-}$. It was observed from open circuit potential (OCP) transients that the potential initially decreased before gradually increasing again in the solutions containing only $CO{_3}^{2-}$ or $PO{_4}^{3-}$ ions, indicating the dissolution or transformation of the native air-formed oxide film into new more protective surface films. The Nyquist plots obtained from electrochemical impedance spectroscopy (EIS) showed that there was growth of new surface films with immersion time on the air-formed oxide film-covered specimens in all the electrolytes; the least resistive surface films were formed in fluoride and sulphate baths whereas the most protective film was formed in phosphate bath. The potentiodynamic polarization curves illustrated that passive behaviour of AZ31 Mg alloy under anodic polarization appears only in $CO{_3}^{2-}$ or $PO{_4}^{3-}$ ions containing solutions and at more than $-0.4V_{Ag/AgCl}$ in $F^-$ ion containing solution.

• 한국표면공학회:학술대회논문집
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• 한국표면공학회 2016년도 추계학술대회 논문집
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• pp.152-152
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• 2016

Anodizing is a technology to generate thicker and high-quality films than natural oxide films by treating metals via electrochemical methods. It is a technique to develop metals for various uses, and extensive research on the commercial use has been performed for a long time. Aluminum anodic oxide (AAO) is generate oxide films, whose sizes and characteristics depending on the types of electrolytes, voltages, temperatures and time. Electrochemical manufacturing method of nano structure is an efficient technology in terms of cost reduction, high productivity and complicated shapes, which receives the spotlight in diverse areas. The sulfuric acid was used as an anodizing electrolyte, controlling its temperature to $10^{\circ}C$. The anode was 5083 Al alloy with dimension of $5(t){\times}20{\times}20mm$ while the cathode was the platinum. The distance between the anode and the cathode was maintained at 3 cm. Agitation was introduced by magnetic stirrer at 300 rpm to prevent localized temperature rise that hinders stable growth of oxide layer. In order to observe surface characteristics with applied current density, the electrolyte temperature, concentration was maintained at constant condition for $10^{\circ}C$, 10 vol.%, respectively. To prevent hindrance of stable growth of oxide layer due to local temperature increase during the experiment, stirring was maintained at constant rate. In addition, using galvanostatic method, it was maintained at current density of $10{\sim}30mA/cm^2$ for 40 minutes. The cavitation experiment was carried out with an ultrasonic vibratory apparatus using piezo-electric effect with modified ASTM-G32. The peak-to-peak amplitude was $30{\mu}m$ and the distance between the horn tip and specimen was 1 mm. The specimen after the experiment was cleaned in an ultrasonic, dried in a vacuum oven for more than 24 hours, and weighed with an electric balance. The surface damage morphology was observed with 3D analysis microscope. As a result of the investigation, differences were observed surface hardness and anti-cavitation characteristics depending on the development of oxide film with applied current density.

• 마이크로전자및패키징학회지
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• 제26권1호
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• pp.35-39
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• 2019

현재까지 다공성 알루미나 구조물은 대표적으로 양극산화 방법으로 구현되어 오고 있다. 양극산화 방법을 통해 규칙적인 배열을 가진 알루미늄 산화 피막은 쉽게 만들 수 있지만, 복합 구조물 형태를 가진 산화피막은 상대적으로 구현하기가 어렵다. 본 연구는 인산용액에서 양극산화 인가전압에 따른 피막 기공 크기, 두께 및 구조물 형태 변화를 관찰하고자 한다. 다층 복합 산화물 구조물 구현을 위해 양극산화 인가전압 조건을 조절하였고, 실험 조건은 10% 인산용액에서 양극산화 인가전압 100 V와 120 V로 각각 수행하였다. 실험 결과는 각 조건에 따라 다공성 구조물과 복합 구조물 형태의 산화물 구조를 구현할 수 있었다.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2016년도 제50회 동계 정기학술대회 초록집
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• pp.407.1-407.1
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• 2016

Electrochromism is defined as a phenomenon which involves persistently repeated change of optical properties between bleached state and colored state by simultaneous injection of electrons and ions, sufficient to induce an electrochemical redox process. Due to this feature, considerable progress has been made in the synthesis of electrochromic (EC) materials, improvements of EC properties in EC devices such as light shutter, smart window and variable reflectance mirrors etc. Among the variable EC materials, solid-state inorganics in particular, metal oxide semiconducting materials such as nickel oxide (NiO) have been investigated extensively. The NiO that is an anodic EC material is of special interest because of high color contrast ratio, large dynamic range and low material cost. The high performance EC devices should present the use of standard industrial production techniques to produce films with high coloration efficiency, rapid switching speed and robust reversibility. Generally, the color contrast and the optical switching speed increase drastically if high surface area is used. The structure of porous thin film provides a specific surface area and can facilitate a very short response time of the reaction between the surface and ions. The large variety of methods has been used to prepare the porous NiO thin films such as sol-gel process, chemical bath deposition and sputtering. Few studies have been reported on NiO thin films made by using sol-gel method. However, compared with dry process, wet processes that have the questions of the durability and the vestige of bleached state color limit the thin films practical use, especially when prepared by sol-gel method. In this study, we synthesis the porous NiO thin films on the fluorine doped tin oxide (FTO) glass by using sputtering and anodizing method. Also we compared electrical and optical properties of NiO thin films prepared by sol gel. The porous structure is promised to be helpful to the properties enhancement of the EC devices.

• 한국세라믹학회지
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• 제41권12호
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• pp.900-906
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• 2004

현재까지 개발되어 온 고체산화물 연료전지는 전해질로 사용되는 산소이온전도성 산화물의 저온에서의 낮은 전도도로 인해 그 사용영역이 제한되어 왔으며, 기판재료가 연료가스 확산층으로 사용되어야 한다는 점 때문에 저온작동을 위한 박막화 역시 명확한 한계를 가지고 있다. 이러한 문제점은 고도의 평활도를 갖는 균일한 나노기공성 기판재를 도입함으로써 해결될 수 있으며, 본 연구에서는 나노기공성 기판에 비정질 금속박막을 증착/산화하는 방안을 제시한다. 초박막형 성공정으로서, 산화 후 산소이온전도성 산화물을 구성하는 합금 타겟을 장착한 DC-magnetron sputter를 사용하여 $20{\sim}200nm$의 기공크기를 갖는 나노기공성 양극산화 알루미나 기판에 비정질 금속합금막을 형성하여 산화/열처리 과정을 거쳐 초박막 산화물 전해질의 제조공정을 실현하였다. 얻어진 박막의 가스투과특성, 입자/입계의 관찰, 상전이에 따른 결정구조/미세구조변화를 관찰하여 초박막 증착 및 전해질의 나노구조제어에 필요한 제반 기본물성데이터를 확보하였다.

• 한국재료학회지
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• 제14권9호
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• pp.607-613
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• 2004

This study was to investigate the surface properties of electrochemically oxidized Ti-6Al-7Nb alloy by anodic spark discharge technique. Anodizing was performed at current density 30 $mA/cm^2$ up to 300 V in electrolyte solutions containing $DL-{\alpha}$-glycerophosphate disodium salt hydrate($DL-{\alpha}$-GP) and calcium acetate (CA). Hydrothermal treatment was done at $300^{\circ}C$ for 2 hrs to produce a thin outermost layer of hydroxyapatite (HA). The bioactivity was evaluated from HA formation on the surfaces in a Hanks' solution with pH 7.4 at $36.5^{\circ}C$ for 30 days. The size of micropores and the thickness of oxide film increased and complicated multilayer by increasing the spark forming voltage. Needle-like HA crystals were observed on anodic oxide film after the hydrothermal treatment at $300^{\circ}C$ for 2 hrs. When increasing $DL-{\alpha}$-GP in electrolyte composition, the precipitated HA crystals showed the shape of thick and shorter rod. However, when increasing CA, the more fine needle shape HA crystals were appeared. The bioactivity in Hanks' solution was accelerated when the oxide films composed with strong anatase peak with presence of rutile peak. The increase of amount of Ca and P was observed in groups having bioactivity in Hanks' solution. The Ca/P ratio of the precipitated HA layer was equivalent to that of HA crystal and it was closer to 1.67 as increasing the immersion time in Hanks' solution.

• 마이크로전자및패키징학회지
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• 제20권4호
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• pp.13-16
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• 2013

양극산화(anodization)공정으로 제작된 규칙성 나노구조의 다공성 산화알루미늄(Aluminum Anodic Oxide, AAO)는 공정이 적용된 LED 모듈은 비교적 쉽고 경제적이므로 최근 LED용 방열소재로 응용하기 위하여 다양하게 연구가 진행되고 있다. 일반적으로 LED 모듈은 알루미늄/폴리머/구리 회로층으로 구성되며 절연체 역할을 하는 폴리머는 히트스프레더로 구성되어있다. 그러나 열전도도가 낮은 폴리머로 인하여 LED부품의 열 방출이 원활하지 못하므로 LED의 수명단축 및 오작동에 영향을 미친다. 따라서, 본 연구에서는 폴리머 대신 상대적으로 열전도도가 우수한 AAO를 양극산화 공정으로 제작하여 히트스프레더(heat spread)로 사용하였다. 이때, AAO와 금속인 구리 회로층간의 접착력을 향상시키기 위하여 스퍼터링 DBC(direct bonding copper)법으로 시드층(seed layer)을 형성한 뒤 최종적으로 전해도금공정으로 구리회로층을 형성하였다. 본 연구에서는 양극 산화공정으로 AAO와 금속간의 접착강도를 개선하여 1.18~1.45 kgf/cm와 같은 우수한 peel strength 값을 얻었다.