• 제목/요약/키워드: EQCM

검색결과 38건 처리시간 0.022초

금속 침출연구를 위한 전기화학적 미소수정진동자저울 기술 소개 (Introduction to Electrochemical Quartz Crystal Microbalance Technique for Leaching Study of Metals)

  • 김민석;정경우;이재천
    • 자원리싸이클링
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    • 제29권1호
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    • pp.25-34
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    • 2020
  • 전기화학적 미소수정진동자저울은 전극표면에서 발생하는 나노그램 수준의 질량변화를 실시간 측정할 수 있는 장비이다. 역압전효과를 가진 수정진동자 양면에 형성된 금속전극에 교대로 전계를 가하면 진동자의 두께에 따라 특정 공진주파수를 나타낸다. 공진주파수는 전극표면에서 발생하는 질량변화에 반응하며, 전극표면의 금속이 용해될 때는 증가하고 석출될 때는 반대로 감소한다. 공진주파수와 질량변화의 상관관계는 Sauerbrey 식으로 나타내고 이를 이용하여 금속의 침출반응때 발생하는 질량변화를 실시간으로 측정할 수 있다. 특히 용해 후 침출액에서 침전, 휘발, 기타 화합물 형성 등 부반응으로 실험 후 발광분광분석이나 원자흡광분석 등이 용이하지 않은 금속의 침출 반응기구 및 속도 연구에 매우 효과적이다. 그러나 수정진동자의 공진주파수는 질량변화 외에도 용액의 점도, 수압, 온도, 스트레스, 그리고 표면거칠기 등에도 영향을 받으므로 실험 시 이들 영향에 대한 고려가 필요하다. 전기화학적 미소수정진동자저울의 응용 예로서 염소를 이용한 백금의 침출 시 용해속도를 실시간 측정하고 이로부터 활성화에너지를 구하는 일련의 과정을 소개하였다. 침출에 사용된 백금시료는 수정진동자 양면에 형성된 1000 Å두께의 백금전극 중 침출액에 노출된 한쪽 면을 활용하였으며, 전해생성된 염소를 염산 침출액에 주입하여 침출 시 용존 염소농도를 조절하였다. 실험결과로부터 염소에 의한 백금의 용해반응은 활성화에너지가 83.5 kJ/mol로 화학반응율속임을 확인하였다.

Electrodeposition of Cu2Se Semiconductor Thin Film on Se-Modified Polycrystalline Au Electrode

  • Lee, Wooju;Myung, Noseung;Rajeshwar, Krishnan;Lee, Chi-Woo
    • Journal of Electrochemical Science and Technology
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    • 제4권4호
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    • pp.140-145
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    • 2013
  • This study describes the electrodeposition of $Cu_2Se$ thin films with a two-step approach that is based on the initial modification of polycrystalline Au electrode with a selenium overlayer followed by a cathodic stripping of the layer as $Se^{2-}$ in a 1 M lactic acid electrolyte containing $Cu^{2+}$ ions. For this two-step approach to be effective, the $Cu^{2+}$ reduction potential should be shifted to more negative potentials passed potentials for the reduction of Se to $Se^{2-}$. This was accomplished by the complexation of $Cu^{2+}$ ions with lactic acid. The resultant $Cu_2Se$ films were characterized by linear sweep voltammetry combined with electrochemical quartz crystal microgravimetry, UV-vis absorption spectrometry and Raman spectroscopy. Photoelectrochemical experiments revealed that $Cu_2Se$ synthesized thus, behaved as a p-type semiconductor.

Detection for folding of the thrombin binding aptamer using label-free electrochemical methods

  • Cho, Min-Seon;Kim, Yeon-Wha;Han, Se-Young;Min, Kyung-In;Rahman, Md. Aminur;Shim, Yoon-Bo;Ban, Chang-Ill
    • BMB Reports
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    • 제41권2호
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    • pp.126-131
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    • 2008
  • The folding of aptamer immobilized on an Au electrode was successfully detected using label-free electrochemical methods. A thrombin binding DNA aptamer was used as a model system in the presence of various monovalent cations. Impedance spectra showed that the extent to which monovalent cations assist in folding of aptamer is ordered as $K^+$ > $NH_4^+$ > $Na^+$ > $Cs^+$. Our XPS analysis also showed that $K^+$ and $NH_4^+$ caused a conformational change of the aptamer in which it forms a stable complex with these monovalent ions. Impedance results for the interaction between aptamer and thrombin indicated that thrombin interacts more with folded aptamer than with unfolded aptamer. The EQCM technique provided a quantitative analysis of these results. In particular, the present impedance results showed that thrombin participates a folding of aptamer to some extent, and XPS analysis confirmed that thrombin stabilizes and induces the folding of aptamer.

A Study on the Capacity Fading and the Replacement of Surface Film at the Surface of $LiMn_2O_4$ Thin Film Electrode

  • Chung Kyung Yoon;Shu Dong;Kim Kwang-Bum
    • 한국전기화학회:학술대회논문집
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    • 한국전기화학회 2002년도 전지기술심포지움
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    • pp.57-65
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    • 2002
  • The presence of tetragonal phase at the surface of $LiMn_2O_4$ pinicle due to a Jahn-Teller offset was previously reported to be one of the causes for capacity fading observed during cycling of $Li//Li_xMn_2O_4$ in 4V range. Further, it is reported that a Jahn-Teller effect in 4V range may be suppressed by substitution of Mn ions with Li ions or other transition metal ions. However, the direct evidence of the suppression of a Jahn-Teller effect in 4V range by substitution of Mn ions with other metal ions has not been reported. The dissolution and formation of surface film at the surface of $LiMn_2O_4$ electrodes also reportedly affect the capacity fading or rate capability. This study reports on the evidence of the onset and suppression of a Jahn-Teller effect in 4V range and the dissolution and formation of surface film at the surface of $LiMn_2O_4$ thin film electrodes using in situ bending beam method (BBM) in situ electrochemical quartz crystal microbalance (EQCM).

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Electrodeposition of Ternary CdZnS Semiconductor Thin Films Using a S-Modified Polycrystalline Au Electrode

  • Ham, Sun-Young;Cho, Se-Jin;Lee, Ung-Ki;Jeon, So-Yeon;Shin, Ji-Cheol;Myung, No-Seung;Paeng, Ki-Jung
    • 전기화학회지
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    • 제10권4호
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    • pp.262-264
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    • 2007
  • This paper describes a two-step approach for the electrochemical deposition of CdZnS thin films on the polycrystalline Au electrode. Initially, an Au substrate is electrochemically modified with a sulfur layer. In the second step, the layer is electroreduced to $S^{2-}$ in the electrolyte dosed with the requisite amount of $Cd^{2+}$ and $Zn^{2+}$ ions to generate CdZnS films in situ. This approach was validated using a combination of linear sweep voltammetry and electrochemical quartz crystal microgravimetry. Thus synthesized CdZnS thin films have different composition depending on the composition of electrolytes. CdZnS thin films are characterized by energy-dispersive X-ray analysis and Raman spectroscopy.

Investigation of the Effect of Acidity and Polyethylene Glycol on Electrochemical Deposition of Trivalent Chromium Ions

  • Phuong, N.V.;Kwon, S.C.;Lee, J.Y.;Kim, M.;Lee, Y.I.
    • 한국표면공학회:학술대회논문집
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    • 한국표면공학회 2011년도 춘계학술대회 및 Fine pattern PCB 표면 처리 기술 워크샵
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    • pp.47-48
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    • 2011
  • The effect of solution acidity and organic additives, polyethylene glycol (PEG), on the trivalent chromium electroplating was systematically investigated in the view point of solution stability, electroreduction of trivalent chromium ions and characterization of deposition layer. It was found that, the concentration of fraction chromium complexes in the trivalent chromium bath containing formic acid is strongly depended on pH value. PEG molecules were stable in trivalent chromium bath containing formic acid via studies on electrospray ionization mass spectrometry (ESI-MS) and UV-Vis. However, the presence of PEG molecules decreased the reductive current of hydrogen evolution, increasing of current efficiency higher about 10 % compared with solutions without PEG. Moreover, PEG additives developed the nodular morphology during electroreduction of trivalent chromium ions with the increase of solution acidity and enhanced its current efficiency by maintaining the consumption of complexant, formic acid, at a low speed. In this study, the effect of solution acidity was emphasized important, there, it controlled the formation of complexes in the solution, cathodic film (CF) during deposition, and properties of deposited layer. By electrochemical quartz crystal microbalance (EQCM), studies show that chromium electrodeposition occurs via the formation of intermediate complexes and adsorption on the cathode surface, which hinder the penetration of ions from bulk solution to the cathode surface.

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도파민으로 수식된 3,4-dihydroxybenzoic acid 고분자 피막전극을 이용한 Ti(IV)이온의 정량 (Poly-3,4-dihydroxybenzoic Acid Film Electrodes Modified with Dopamine for Determination of Ti(IV) Ions)

  • 차성극
    • 전기화학회지
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    • 제6권2호
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    • pp.130-133
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    • 2003
  • 3,4-dihydroxybenzoic acid(3,4-DHBA)를 전기화학법으로 유리탄소 전극 위에 중합하여 GC/p-3,4-DHBA형의 전극을 제작한 후 이 전극을 도파민으로 재 수식한 전극을 제작하였다. 이 때 고분자 피막 상에 카르복시기와 도파민의 아민 기간에 짝 짓기 반응은 1-(3-dimethylaminopropyl)-3-ethyl carbodiimide hydrochloride(EDC)의 존재하에서 진행되었다. 이 반응과정에서 반응한 도파민의 양은 수정판 분석기(quartz crystal analyzer:QCA)에 의하여 결정하였으며 그때 전극형태는 QCA(Au)/p-3,4-DHBA-dopamine이었다. 이 전극의 표면은 o-퀴논부분을 갖고 있어서 티탄이온에 선택성이 큰 특성을 갖고 있다. 이 전극의 산화환원과정은 $hydroquinone = quinone +2H^+2e^-$으로 두 개의 강한 파와 두개의 약한 파가 CV과정에서 관찰되었다. 이 수식전극으로 Ti(IV)이온을 $4.13\times10^{-5} gcm^{-2}$만큼 포집할 수가 있었다. 이 수식 전극으로 $5.25\times10^{-4}M$에서 $5.25\times10^{-8}M$농도범위까지 정량 할 수 있는 상관계수가 0.997인 검정선을 얻었다.

3가크롬 이온의 전착 반응에 용액 산도 및 유기물 첨가제가 미치는 영향 연구 (Investigation of the Effect of Solution Acidity and Organic Additives on the Electrodeposition of Trivalent Chromium Ions)

  • 이주열;;강대근;김만;권식철
    • 한국표면공학회지
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    • 제43권6호
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    • pp.297-303
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    • 2010
  • The effect of solution acidity and organic additives, polyethylene glycol (PEG), on the trivalent chromium electroplating was systematically investigated in the view point of electroreduction of trivalent chromium ions and solution stability. It was found that solution acidity controlled at pH 2.5 showed the widest current range for bright electrodeposits in the presence of PEG additives, which reduced the local current intensification at high current densities. Through complex interaction between PEG additives and hydrogen ion, that is, solution acidity, electrode potential was moved in the negative direction in the bulk solution, while it shifted in the positive when electric potential was scanned. In conjunction with electrochemical quartz crystal microbalance (EQCM), it was found that PEG additives had a role in promoting the electron transfer to trivalent chromium ion complexes in bulk solution and their adsorption at the electrode surface as well as interfering with hydrogen ion reduction process below pH 2.5. The PEG additives developed the nodular morphology during electroreduction of trivalent chromium ions with the increase of solution acidity and enhanced its current efficiency by maintaining the consumption of complexant, formic acid, at low speed.