• Title, Summary, Keyword: Microbalance

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Electrochemistry for Redox Polymer Film of N,N'-bis(3-pyrrol-1-yl-propyl)-4,4'-bipyridinium Ion (N,N'-bis(3-pyrrol-1-yl-propyl)-4,4'-bipyridinium이온의 산화-환원 고분자 피막에 대한 전기화학)

  • Cha, Seong-Keuck
    • Polymer Korea
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    • v.25 no.1
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    • pp.6-14
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    • 2001
  • The monomer N,N'-bis(3-pyrrol-1-yl-propyl)-4,4'-bipyridinium$(PF_6)_2$ was electrochemically polymerized on glassy carbon electrode surface. This polymer film electrode has electroactive sites on its bipyridinium ions distributed at the polymer strands. The formal potentials of the electrodes were -0.41V and -0.81V(vs. SSCE) for each step at phosphate buffer(pH=5.70). The diffusion coefficients of the dopants ions into the polymer matrix were $1.57{\times}10^{-4}$ and $4.35{\times}10^{-5}cm^2s^{-1}$ for first and second redox couple, respectively. The rate constants of electron transfer at $V^{2+/+}$ of the first step was a $57.53s^{-1}$, which was 22 times higher than $V^{+/0}$ one having $2.63s^{-1}$ in the solution. The charge transfer resistance of the polymer film was influenced by the dopant ion of the electrolyte. Thus the resistances were 22.63, 16.81, 12.44 and $11.36k{\Omega}$ for $LiClO_4,\;NaClO_4,\;KClO_4$, and phosphate buffer, respectively. The reaction order of the electropolymerization was first order and the rate constant of the polymerization was $1.31{\times}10^{-1}s^{-1}$ as determined by EQCM method. The G.C./p-BPB type electrode doped with phosphate ions showed a stability and reproducibility in CV procedure over 20 cycles.

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Fabrication of TiO2/polyelectrolyte thin film for a methyl mercaptan gas sensor (메칠멜캅탄 가스센서용 TiO2/전해질폴리머 박막 제조)

  • Kim, Jin-Ho;Hwang, Jong-Hee;Lee, Mi-Jai;Kim, Sei-Ki;Lim, Tae-Young
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.20 no.5
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    • pp.221-226
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    • 2010
  • Quartz crystal microbalance (QCM) gas sensor to detect methyl mercaptan ($CH_3SH$) gas was fabricated by depositing $TiO_2$ nanoparticles and polyelectrolyte on the electrode of QCM. The $TiO_2$/poly(sodium 4-styrenesulfonate) (PSS) thin film fabricated by a layer-by-layer self-assembly (LBL-SA) method showed a high surface area and increased the sensitivity of gas sensor. When the QCM sensors coated with triethanolamine (TEA) or ($TiO_2$/PSS) were exposed to methyl mercaptan gas (1.0 ppm), the frequency shifts of QCM with TEA casting film and $TiO_2$/PSS thin film were ca. 9 Hz and ca. 24 Hz, respectively. As the bilayer number of ($TiO_2$/PSS) increased, the frequency shift of QCM sensor with ($TiO_2$/PSS) thin film was gradually increased. In addition, the frequency shift of QCM sensor was gradually increased as the concentration of methyl mercaptan gas increased from 0.5 ppm to 2.0 ppm. In this study, the surface morphology and sensor property of QCM sensor coated with ($TiO_2$/PSS) thin film were measured.

Fabrication of functional nanoparticles by layer-by-layer self-assembly method (LBL 법을 이용한 기능성 나노 입자 제조)

  • Kim, Jin-Ho;Hwang, Jong-Hee;Lim, Tae-Young;Kim, Sae-Hoon
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.19 no.6
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    • pp.305-310
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    • 2009
  • $TiO_2$ thin films consisting of positively charged poly (diallyldimethylammonium chloride) (PDDA) and negatively charged titanium (IV) bis (ammonium lactato) dihydroxide (TALH) were successfully fabricated on a poly (methyl methacrylate) (PMMA) by layer-by-layer (LBL) self-assembly method. By the measurement of quartz crystal microbalance (QCM), it was found that as the solution pH of TALH decreased, the deposition volume of TALH increased and the thickness of (PDDA/TALH) thin film coated on the surface of PMMA particles increased. The PMMA particles coated with the coating sequence of (PDDA/TALH)n showed the variation of color changes as a function of the number of bilayer. The number of bilayer (n) of (PDDA/TALH) thin films was 10 and 20, the values of $a^*$ and $b^*$ decreased from those of PMMA particles without coating films and the color changes was shifted to green and blue direction in the $a^*$, $b^*$ chromaticity diagram. And then, the number of n increased to 30 and 40, the values of $a^*$ and $b^*$ increased and the color changes was shifted to red and yellow direction, respectively. Finally the PMMA particles coated with $(PDDA/TALH)_{50}$ thin film showed a little same value of $a^*$ and $b^*$ with the PMMA particles without (PDDA/TALH) thin film.

The Application of Octa-Substituted Metallophthalocyanine Langmuir-Blodgett films for $NO_2$ Measurement (수정진동자를 이용한 프탈로시아닌 LB박막의 $NO_2$ 감지 특성)

  • Kwon, H.J.;Lee, Y.J.;Chang, Y.K.;Kim, J.D.
    • Journal of Sensor Science and Technology
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    • v.7 no.4
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    • pp.254-262
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    • 1998
  • Multilayer Langmuir-Blodgett (LB) films coated on quartz crystal microbalance (QCM) of octa-substituted metallophhtalocyanines ($MPc(OEH)_8$, M = Cu, Co, and Sn) and dihydrogen phthalocyanines ($H_2Pc(OEH)_8$) were used to quantify $NO_2$ concentrations. They were exposed to various concentrations of $NO_2$ in dry $N_2$. Among the four phthalocyanines we tested, the metal-free $H_2Pc(OEH)_8$ was observed to be most sensitive to $NO_2$. However, its LB film showed a partially irreversible behavior, that is part of the frequency change due to $NO_2$ adsorption could not be recovered even after purging with pure $N_2$ gas for an extended period. Examining the spectra of NMR and FTIR revealed fact that the irreversible portion of frequency change was due to ether groups in the linkage between side chains and the Pc unit. In order to remove the effect of such initial deactivation, on $NO_2$ quantification experiment, a freshly fabricated LB film was treated at a high concentration of $NO_2$ so that the ether sites were saturated. A pretreated LB film showed a reproducible performance for repeated uses. The $CuPc(OEH)_8$ LB film showed a satisfactory sensing performance down to as low as 4 ppm. For the $H_2Pc(OEH)_8$ LB film, the lower detection limit was found to be 35ppb of $NO_2$. In order to make the experimental condition more realistic, the carrier gas, dry nitrogen, was replaced by air. It was observed that the presence of oxygen, a weak electron acceptor, reduced the sensitivity and thus increased the sensing limit to hundreds of ppb. Results of experiments with moisture added showed that the interference of moisture was quite severe.

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Anion Effects on Changes in Viscoelasticity of Polypyrrole during Electrochemical Growth in Neutral Aqueous Solutions (중성 수용액에서 폴리피롤의 전기화학적 성장시 발생하는 점탄성 변화에 미치는 음이온 효과)

  • Bae Sang-Eun;Lee Seung-Yong;Paek Se-Hwan;Kim Young-Sang;Lee Chi-Woo
    • Journal of the Korean Electrochemical Society
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    • v.2 no.2
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    • pp.66-69
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    • 1999
  • A large number of works have been Performed to understand the electrochemical growth of Polypynole on conducting substrates in aqueous as well as in nonaqueous solutions. Recently most researches with Polypyrrole have tended to be directed toward technological applications, but many fundamental physical and chemical properties of Polypyrrole remain unknown. In Particular, microrheological Property of polypyrrole has been largely neglected until the advanced electrochemical quartz crystal microbalance technique was introduced recently. To study anion effects on microrheolosical Property of Polypyrrole, we investigated changes in viscoelasticity of Polypyrrole during electrochemical growth in neutral aqueous solutions by means of in siか electrochemical quartz crystal oscillator method. The results showed that the films of Polypyrrole synthesized in $KPF_6\;and\;KCIO_4$ were more viscoelastic than the ones in $KCI,\;KNO_3,\;KBr,\;KBF_4,\;K_2SO_4$, sodium tosylate (NaOTs), and sodium dodecyl sulfate (SDS). The growth rate of Polypyrrole in SDS was faster than that in the others utilized. Polypyrroles synthesized in buffered neutral solutions were more elastic than those in unbuffered neutral solutions.