• Title/Summary/Keyword: Electrochemical polishing

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나노 구조의 $CeO_2$ 합성과 전기화학적 특성 분석 (Synthesis and electrochemical characterization of nano structure $CeO_2$)

  • 조민영;이재원;박선민;노광철;최헌진
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2009년도 하계학술대회 논문집
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    • pp.462-462
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    • 2009
  • $CeO_2$는 고체 산화물 연료전지 (SOFC, soild oxide fuel cell)의 전해질 재료와 CMP(Chemical Mechanical Polishing) 슬러리 재료, 자동차의 3원 촉매, gas sensor, UV absorbent등 여러 분야에서 사용되고 있다. 본 연구에서는 위의 활용범위 외에 $CeO_2$의 구조적 안정성과 빠른 $Ce^{3+}/Ce^{4+}$의 전환 특성을 이용하여 lithium ion battery의 anode 재료로서 전기화학적 특성을 알아보고자 실험을 실시하였다. $CeO_2$ 합성에 사용되는 전구체인 cerium carbonate의 형상 및 크기, 비표면적과 같은 물리화학적 특성이 $CeO_2$ 분말의 특성에 직접적인 영향을 주기 때문에 전구체의 합성 단계에서 입자의 특성을 조절하였다. 전구체 합성의 출발원료로 cerium nitrate hexahydrate 와 ammonium carbonate를 사용하였고 반응온도 및 농도 등을 변화시켜 입자의 형상 및 결정상을 fiber형태의 orthorombic $Ce_2O(CO_3)_2{\cdot}H_2O$와 구형의 hexagonal $CeCO_3OH$의 세리아 전구체를 합성하였다. 이를 $300^{\circ}C$에서 30분 동안 하소하여 전구체의 입자형상을 유지하는 cubic $CeO_2$를 합성하고 X-ray diffraction, FE-SEM, micropore physisorption analyzer 분석을 통하여 입자의 결정상과 형상, 비표면적 등을 비교 분석하고 $Li/CeO_2$ couple의 충,방전 용량과 수명특성을 비교 분석하여 $CeO_2$의 전기화학적 특성을 알아보았다.

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치과용 아말감의 산화환원에 관한 전기화학적 연구 (AN ELECTROCHEMICAL STUDY ON THE OXIDATION' AND REDUCTION OF DENTAL AMALGAM)

  • 이인복;이명종
    • Restorative Dentistry and Endodontics
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    • 제18권2호
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    • pp.431-445
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    • 1993
  • The purpose of this study was to observe corrosion characteristics of six dental amalgams and was to analyse corrosion products electrochemically. After each amalgam alloy and Hg was triturated as the direction of the manufacturer by using mechanical amalgamator, the triturated mass was inserted into the cylinderical metal mold ($12{\times}10mm$) and was condensed with 160kg/$cm^2$ by using the hydrolic press. The specimen was removed from the mold and was stored at room temperature for 1 week, and was polished with amalgam polishing kit. The anodic and cathodic polarization curve was obtained by using cyclic voltammetric method with 3-electrode potentiostat in saline for each amalgam and Ag, Sn, Cu plate specimen at $37{\pm}0.5^{\circ}C$. The potential sweep range was -1.7V~0. 4V(vs SCE) in working electrode and scan rate was 50mV/s and the exposed surface area of each specimen to the electrolytic solution was $0.79cm^2$. The results were as follows. 1. In anodic-cathodic polarization curve of amalgam specimens, two anodic current rising areas and two cathodic current peaks were obtained at the low Cu amalgam(CF, CS) specimen and three anodic current rising areas and three cathodic current peaks were obtained at the high Cu amalgam (TY, DS, HV) specimen. 2. As this compared with the anodic and cathodic current peak potentials of Sn, Cu and Ag specimen, the first cathodic current peak I c was caused by the reduction of divalent tin salt, second cathodic current peak IIIc results from the reduction of quadravalent tin salt, and third cathodic current peak me results from the reduction of copper salt. 3. As reverse potential sweeping was done repeatedly, anodic current was decreased slightly in all amalgam specimens.

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Al2O3 산화 피막의 내식성에 미치는 양극산화 전류밀도의 영향 (Effect of Anodizing Current Density on Anti-Corrosion Characteristics for Al2O3 Oxide Film)

  • 이승준;장석기;김성종
    • 한국표면공학회:학술대회논문집
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    • 한국표면공학회 2016년도 추계학술대회 논문집
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    • pp.153-153
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    • 2016
  • Aluminum alloys have poor corrosion resistance compared to the pure aluminum due to the additive elements. Thus, anodizing technology artificially generating thick oxide films are widely applied nowadays in order to improve corrosion resistance. Anodizing is one of the surface modification techniques, which is commercially applicable to a large surface at a low price. However, most studies up to now have focused on its commercialization with hardly any research on the assessment and improvement of the physical characteristics of the anodized films. Therefore, this study aims to select the optimum temperature of sulfuric electrolyte to perform excellent corrosion resistance in the harsh marine environment through electrochemical experiment in the sea water upon generating porous films by variating the temperatures of sulfuric electrolyte. To fabricate uniform porous film of 5083 aluminum alloy, we conducted electro-polishing under the 25 V at $5^{\circ}C$ condition for three minutes using mixed solution of ethanol (95 %) and perchloric (70 %) acid with volume ratio of 4:1. Afterward, the first step surface modification was performed using sulfuric acid as an electrolyte where the electrolyte concentration was maintained at 10 vol.% by using a jacketed beaker. For anode, 5083 aluminum alloy with thickness of 5 mm and size of $2cm{\times}2cm$ was used, while platinum electrode was used for cathode. The distance between the two was maintained at 3 cm. Afterward, the irregular oxide film that was created in the first step surface modification was removed. For the second step surface modification process (identical to the step 1), etching was performed using mixture of chromic acid (1.8 wt.%) and phosphoric acid (6 wt.%) at $60^{\circ}C$ temperature for 30 minutes. Anodic polarization test was performed at scan rate of 2 mV/s up to +3.0 V vs open circuit potential in natural seawater. Surface morphology was compared using 3D analysis microscope to observe the damage behavior. As a result, the case of surface modification presented a significantly lower corrosion current density than that without modification, indicating excellent corrosion resistance.

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Sodium Periodate 기반 Slurry의 pH 변화가 Ru CMP에 미치는 영향 (Effect of pH in Sodium Periodate based Slurry on Ru CMP)

  • 김인권;조병권;박진구
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2008년도 하계학술대회 논문집 Vol.9
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    • pp.117-117
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    • 2008
  • In MIM capacitor, poly-Si bottom electrode is replaced with metal bottom electrode. Noble metals can be used as bottom electrodes of capacitors because they have high work function and remain conductive in highly oxidizing conditions. In addition, they are chemically very stable. Among novel metals, Ru (ruthenium) has been suggested as an alternative bottom electrode due to its excellent electrical performance, including a low leakage of current and compatibility to high dielectric constant materials. Chemical mechanical planarization (CMP) process has been suggested to planarize and isolate the bottom electrode. Even though there is a great need for development of Ru CMP slurry, few studies have been carried out due to noble properties of Ru against chemicals. In the organic chemistry literature, periodate ion ($IO_4^-$) is a well-known oxidant. It has been reported that sodium periodate ($NaIO_4$) can form $RuO_4$ from hydrated ruthenic oxide ($RuO_2{\cdot}nH_2O$). $NaIO_4$ exist as various species in an aqueous solution as a function of pH. Also, the removal mechanism of Ru depends on solution of pH. In this research, the static etch rate, passivation film thickness and wettability were measured as a function of slurry pH. The electrochemical analysis was investigated as a function of pH. To evaluate the effect of pH on polishing behavior, removal rate was investigated as a function of pH by using patterned and unpatterned wafers.

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텅스텐 화학적-기계적 연마 공정에서 부식방지막이 증착된 금속 컨디셔너 표면의 전기화학적 특성평가 (Electrochemical Characterization of Anti-Corrosion Film Coated Metal Conditioner Surfaces for Tungsten CMP Applications)

  • 조병준;권태영;김혁민;;박문석;박진구
    • 마이크로전자및패키징학회지
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    • 제19권1호
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    • pp.61-66
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    • 2012
  • 반도체 산업에서 회로의 고집적화와 다층구조를 형성하기 위해 화학적-기계적 연마(CMP: Chemical-Mechanical Planarization) 공정이 도입되었으며 반도체 패턴의 미세화와 다층화에 따라 화학적-기계적 연마 공정의 중요성은 더욱 강조되고 있다. 화학적-기계적 연마공정이란 화학적 반응과 기계적 힘을 동시에 이용하여 표면을 평탄화하는 공정으로, 화학적-기계적 연마 공정은 압력, 속도 등의 공정조건과, 화학적 반응을 유도하는 슬러리(Slurry), 기계적 힘을 위한 패드 등에 의해 복합적으로 영향을 받는다. 패드 컨디셔닝이란 컨디셔너가 화학적-기계적 연마 공정 중에 지속적으로 패드 표면을 연마하여 패드의 손상된 부분을 제거하고 새로운 표면을 노출시켜 패드의 상태를 일정하게 유지시키는 것을 말한다. 한편, 금속박막의 화학적-기계적 연마 공정에 사용되는 슬러리는 금속박막과 산화반응을 하기 위하여 산화제를 포함하는데, 산화제는 금속 컨디셔너 표면을 산화시켜 부식을 야기한다. 컨디셔너의 표면부식은 반도체 수율에 직접적인 영향을 줄 수 있는 스크래치(Scratch) 등을 발생시킬 뿐만 아니라, 컨디셔너의 수명도 저하시키게 되므로 이를 방지하기 위한 노력이 매우 중요하다. 본 연구에서는 컨디셔너 표면에 슬러리와 컨디셔너 표면 간에 일어나는 표면부식을 방지하기 위하여 유기박막을 표면에 증착하여 부식을 방지하고자 하였다. 컨디셔너 제작에 사용되는 금속인 니켈과 니켈 합금을 기판으로 하고, 증착된 유기박막으로는 자기조립단분자막(SAM: Self-Assembled Monolayer)과 불화탄소(FC: FluoroCarbon) 박막을 증착하였다. 자기조립단분자막은 2가지 전구체(Perfluoroctyltrichloro silane(FOTS), Dodecanethiol(DT))를 사용하여 기상 자기조립 단분자막 증착(Vapor SAM) 방법으로 증착하였고, 불화탄소막은 10 nm, 50 nm, 100 nm 두께로 PE-CVD(Plasma Enhanced-Chemical Vapor Deposition, SRN-504, Sorona, Korea) 방법으로 증착하여 표면의 부식특성을 평가하였다. 표면 부식 특성은 동전위분극법(Potentiodynamic Polarization)과 전기화학적 임피던스 측정법(Electrochemical Impedance Spectroscopy(EIS)) 등의 전기화학 분석법을 사용하여 평가되었다. 또한 측정된 임피던스 데이터를 전기적 등가회로(Electrical Equivalent Circuit) 모델에 적용하여 부식 방지 효율을 계산하였다. 동전위분극법과 EIS의 결과 분석으로부터 유기박막이 증착된 표면의 부식전류밀도가 감소하고, 임피던스가 증가하는 것을 확인하였다.