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GLAD법으로 증착한 Smart window용 WO3와 TiO2의 전기변색적 특성 비교

  • Kim, Seong-Han;Song, Pung-Geun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2015.08a
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    • pp.198-198
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    • 2015
  • 전기변색재료는 전압을 인가하였을 때 전계방향에 따라 가역적으로 색이 변화하는 재료를 말한다. 스마트윈도우용 전기 변색재료는 지속적으로 전기를 가해줄 필요 없이 한번 변색되면 색이 지속되는 특징을 가지므로 에너지 효율적으로 우수하여 태양열 차단 창호나 디스플레이 분야에 응용될 것으로 기대된다. 이러한 전기 변색재료에는 산화형 전기 변색 재료, 환원형 전기 변색 재료가 있는데 이중 가장 널리 연구되고 있는 재료는 환원형 전기변색재료이다. 대표적인 재료로 $WO_3$가 쓰이는 데 이는 전기 변색적 특성이 우수하고 또한 내구성이 다른 재료에 비해 우수하다는 장점 때문이다. 그러나, 상용화를 위해서는 내구성의 개선이 요구되고 있다. 한편, $TiO_2$는 안정성이 매우 뛰어나지만 전기변색적 특성이 $WO_3$에 비해 낮은 점이 지적되고 있다. 이러한 $WO_3$$TiO_2$ 박막은 스퍼터링 또는 sol-gel법 등으로 제작되고 있는데, 일반적으로 스퍼터링의 경우 치밀한 박막이 형성되기 때문에 Porous 한 박막을 얻기 힘들다. 따라서 본 연구에서는 기판에 입사하는 스퍼터 입자들의 각도를 조절하여 shadowing 효과로 인해 박막의 구조가 porous해지는 Glancing angle deposition을 도입하였다. 이러한 증착법을 이용하여 $WO_3$$TiO_2$를 각도를 조절하여 증착하고 $TiO_2$$WO_3$ 박막의 특성을 비교하여 본다. 두께 300 nm를 가지는 $WO_3$$TiO_2$ 박막은 GLAD RF 마그네트론 스퍼터링법을 이용하여 Corning glass(corning E-2000)기판 위에 증착하였다. 기판 입사 각도는 $0^{\circ}$, $30^{\circ}$, $45^{\circ}$, $60^{\circ}$로 증착하였고 직경 3 in의 $TiO_2$, $WO_3$ 타겟을 사용하였다. 또한 스퍼터링 파워는 400 W, 작업압력 1.0 Pa, 그리고 스퍼터링 가스는 O2/Ar+O2 유량 10%에서 30%로 증착을 상온에서 진행하였다. 전기화학적 특성을 평가하기 위하여 $TiO_2$$WO_3$ 박막을 100 nm 두께의 ITO/glass 위에서 증착하였다. 박막의 미세구조는 XRD와 SEM을 통해 확인하였고, 전기화학적 특성은 Ar 분위기의 Glove box안에서 parstat 2273을 통해 측정하였다. 전해질은 1 M $LiPF_6/PC$로 진행하였고, 대향 전극는 Pt전극을, 참고 전극은 칼로멜 전극을 사용하였다. Potential 범위는 2 V에서 4 V로 진행하였고, scan rate는 50 mV/s로 측정하였다. 투과도는 UV/VIS spectrometer로 측정하였다. 전기변색 특성의 상관관계 및 에 대해서는 학회 당일 발표할 예정이다.

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The Study of Color and Hardness of TiN Thin Film by UBM Sputtering System (UBM Sputtering System에 의한 TiN막의 색상과 경도에 관한 연구)

  • Park, Moon Chan;Lee, Jong Geun;Joo, Kyung Bok
    • Journal of Korean Ophthalmic Optics Society
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    • v.14 no.1
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    • pp.57-62
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    • 2009
  • Purpose: TiN films were deposited on sus304 by unbalanced magnetron sputtering system which was designed and developed as unbalancing the strength of the magnets in the magnetron electrode. The color and hardness of deposited TiN films was investigated. Methods: The cross sections of deposited films on silicon wafer were observed by SEM to measure the thickness of the films, the components of the surface of the films were identified by XPS, the components of the inner parts of the films were observed by XPS depth profiling. XPS high resolution scans and curve fittings of deposited films were performed for quantitative chemical analysis, Vickers micro hardness measurements of deposited films were performed with a nano indenter equipment. Results: The colors of deposited films gradually changed from light gold to dark gold, light violet, and indigo color with increasing of the thickness. It could be seen that the color change come from the composite change of three compound,$TiO_{x}N_{y}$, $TiO_2$, TiN. Especially, the composite change of$TiO_{x}N_{y}$ compound was thought to affect the color change with respect to thickness. Conclusions: Deposited films had lower than the value of general TiN film in Vickers hardness, which was caused by mixing three TiN, $TiO_2$,$TiO_{x}N_{y}$ compound in the deposited films. The increasing and decreasing of micro hardness with respect to thickness was thought to have something to do with the composite of TiN in the films.

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MOCVD Growth and Characterization of Heteroepitaxial Beta-Ga2O3 (MOCVD 성장법을 이용한 Beta-Ga2O3 박막의 헤테로에피택시 성장 특성)

  • Jeong Soo Chung;An-Na Cha;Gieop Lee;Sea Cho;Young-Boo Moon;Myungshik Gim;Moo Sung Lee;Jun-Seok Ha
    • Journal of the Microelectronics and Packaging Society
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    • v.31 no.2
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    • pp.85-91
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    • 2024
  • In this study, we investigated a method of growing single crystal 𝛽-Ga2O3 thin films on a c-plane sapphire substrate using MOCVD. We confirmed the optimal growth conditions to increase the crystallinity of the 𝛽-Ga2O3 thin film and confirmed the effect of the ratio between O2 and Ga precursors on crystal growth on the crystallinity of the thin film. The growth temperature range was 600~1100℃, and crystallinity was analyzed when the O2/TMGa ratio was 800~6000. As a result, the highest crystallinity thin film was obtained when the molar ratio between precursors was 2400 at 1100℃. The surface of the thin film was observed with a FE-SEM and XRD ω-scan of the thin film, the FWHM was found to be 1.17° and 1.43° at the and (${\bar{2}}01$) and (${\bar{4}}02$) diffraction peaks. The optical band gap energy obtained was 4.78 ~ 4.88 eV, and the films showed a transmittance of over 80% in the near-ultraviolet and visible light regions.

A STUDY ON IN VIVO AND IN VITRO AMALGAM CORROSION (아말감의 구강내 부식 및 인공 부식에 관한 연구)

  • Lim, Byong-Mok;Kwon, Hyuk-Choon;Um, Chung-Moon
    • Restorative Dentistry and Endodontics
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    • v.22 no.1
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    • pp.1-33
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    • 1997
  • The objective of this study was to analyze the in vitro and in vivo corrosion products of low and high copper amalgams. The four different types of amalgam alloy used in this study were Fine cut, Caulk spherical, Dispersalloy, and Tytin. After each amalgam alloy and Hg were triturated according to the directions of the manufacturer by means of the mechanical amalgamator(Amalgam mixer. Shinhung Co. Korea), the triturated mass was inserted into a cylindrical metal mold which was 12mm in diameter and 10mm in height. The mass was condensed by 150Kg/cm compressive force. The specimen was removed from the mold and aged at room temperature for about seven days. The standard surface preparation was routinely carried out by emery paper polishing under running water. In vitro amalgam specimens were potentiostatically polarized ten times in a normal saline solution at $37^{\circ}C$(potentiostat : HA-301. Hukuto Denko Corp. Japan). Each specimen was subjected to anodic polarization scan within the potential range -1700mV to+400mV(SCE). After corrosion tests, anodic polarization curves and corrosion potentials were obtained. The amount of component elements dissolved from amalgams into solution was measured three times by ICP AES(Inductive Coupled Plasma Atomic Emission Spectrometry: Plasma 40. Perkim Elmer Co. U.S.A.). The four different types of amalgam were filled in occlusal and buccal class I cavities of four human 3rd molars. After about five years the restorations were carefully removed after tooth extraction to preserve the structural details including the deteriorated margins. The occlusal surface, amalgam-tooth interface and the fractured surface of in vivo amalgam corrosion products were analyzed. In vivo and in vitro amalgam specimens were examined and analyzed metallographically by SEM(Scanning Electron Microscope: JSM 840. Jeol Co. Japan) and EDAX(Energy Dispersive Micro X-ray Analyser: JSM 840. Jeol Co. Japan). 1. The following results are obtained from in vitro corrosion tests. 1) Corrosion potentials of all amalgams became more noble after ten times passing through the in vitro corrosion test compared to first time. 2) After times through the test, released Cu concentration in saline solution was almost equal but highest in Fine cut. Ag and Hg ion concentration was highest in Caulk spherical and Sn was highest in Dispersalloy. 3) Analyses of surface corrosion products in vitro reveal the following results. a)The corroded surface of Caulk spherical has Na-Sn-Cl containing clusters of $5{\mu}m$ needle-like crystals and oval shapes of Sn-Cl phase, polyhedral Sn oxide phase. b)In Fine cut, there appeared to be a large Sn containing phase, surrounded by many Cu-Sn phases of $1{\mu}m$ granular shapes. c)Dispersalloy was covered by a thick reticular layer which contained Zn-Cl phase. d)In Tytin, a very thin, corroded layer had formed with irregularly growing Sn-Cl phases that looked like a stack of plates. 2. The following results are obtained by an analysis of in vivo amalgam corrosion products. 1) Occlusal surfaces of all amalgams were covered by thick amorphous layers containing Ca-P elements which were abraded by occlusal force. 2) In tooth-amalgam interface, Ca-P containing products were examined in all amalgams but were most clearly seen in low copper amalgams. 3) Sn oxide appeared as a polyhedral shape in internal space in Caulk spherical and Fine cut. 4) Apical pyramidal shaped Sn oxide and curved plate-like Sn-Cl phases resulted in Dispersalloy. 5) In Tytin, Sn oxide and Sn hydroxide were not seen but polyhedral Ag-Hg phase crystal appeared in internal space which assumed a ${\beta}_l$ phase.

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Electrochemical Characteristic on Hydrogen Intercalation into the Interface between Electrolyte of the 0.1N H2SO4and Amorphous Tungsten Oxides Thin Film Fabricated by Sol-Gel Method (졸-겔법으로 제조된 비정질의 텅스텐 산화물 박막과 황산 전해질 계면에서 일어나는 수소의 층간 반응에 대한 전기화학적 특성)

  • Kang, Tae-Hyuk;Min, Byoung-Chul;Ju, Jeh-Beck;Sohn, Tae-Won;Cho, Won-Il
    • Applied Chemistry for Engineering
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    • v.7 no.6
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    • pp.1078-1086
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    • 1996
  • The peroxo-polytungstic acid was formed by the direct reaction of tungsten powder with the hydrogen peroxide solution. Peroxo-polytungstic powder were prepared by rotary evaporator using the fabricated on to ITO coated glass as substrate by dip-coating method using $2g/10mL(W-IPA/H_2O)$ sol solution. A substrate was dipped into the sol solution and after a meniscus had settled, the substrate was withdrawn at a constant rate of the 3mm/sec. Thicker layer could be built up by repeated dipping/post-treatment 15 times cycles. The layers dried at the temperature of $65{\sim}70^{\circ}C$ during the withdrawn process, and then tungsten oxides thin film was formed by final heating treatment at the temperature of $230{\sim}240^{\circ}C$ for 30min. A linear rotation between the thickness of thin film and the number of dipping/post-treatment cycles for tungsten oxides thin films made by dip-coating was found. The thickness of thin film had $60{\AA}$ after one dipping. From the patterns of XRD, the structure of tungsten oxides thin film identified as amorphous one and from the photographs of SEM, the defects and the moderate cracks were observed on the tungsten oxides thin film, but the homogeneous surface of thin films were mostly appeared. The electrochemical characteristic of the $ITO/WO_3$ thin film electrode were confirmed by the cyclic voltammetry and the cathodic Tafel polaization method. The coloring bleaching processes were clearly repeated up to several hundreds cycles by multiple cyclic voltammetry, but the dissolved phenomenon of thin film revealed in $H_2SO_4$ solution was observed due to the decrease of the current densities. The diffusion coefficient was calculated from irreversible Randles-Sevick equation from the data obtained by the cyclic voltammetry with various scan rates.

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