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COMBINATION OF SCANNING ELECTROCHEMICAL MICROSCOPY AND LOCAL ELECTROCHEMICAL IMPEDANCE METHOD

Research Project

Project/Area Number 10555236
Research Category

Grant-in-Aid for Scientific Research (B)

Allocation TypeSingle-year Grants
Section展開研究
Research Field Material processing/treatments
Research InstitutionHOKKAIDO UNIVERSITY

Principal Investigator

SEO Masahiro  Hokkaido Univ., Grad. School of Eng., Asso. Pro., 大学院・工学研究科, 教授 (20002016)

Co-Investigator(Kenkyū-buntansha) FUSHIMI Koji  Hokkaido Univ., Grad. School of Eng., Inst., 大学院・工学研究科, 助手 (20271645)
AZUMI Kazuhisa  Hokkaido Univ., Grad. School of Eng., Asso. Pro., 大学院・工学研究科, 助教授 (60175875)
Project Period (FY) 1998 – 1999
Project Status Completed (Fiscal Year 1999)
Budget Amount *help
¥12,600,000 (Direct Cost: ¥12,600,000)
Fiscal Year 1999: ¥1,300,000 (Direct Cost: ¥1,300,000)
Fiscal Year 1998: ¥11,300,000 (Direct Cost: ¥11,300,000)
KeywordsScanning Electrochemical Microscopy / Local Electrochemical Impedance Method / Local Electrochemical Reaction / Evaluation of Heterogeneity / Passive Film / Iron / Titanium / Combined Probe Electrodes / マイクロインピーダンス測定 / 半導体特性 / 微小白金黒電極
Research Abstract

The combinational use of scanning electrochemical microscopy (SECM) and other micro-electrochemical techniques, such as local electrochemical impedance method (LEIM), scanning droplet cell (SDC) and liquid-phase ion gun, was attempted to evaluate the heterogeneity of electrochemical reaction at the metal and solution interface in a scale of several μm to several ten μm. Furthermore, the performance of SECM was improved to obtain the more precise probe current images. The following results were obtained.
1. Micro-disk platinum electrode for SECM was combined with micro-platinum black electrodes for LEIM. A platinum foil embedded into epoxy resin was used as a model specimen electrode. Both SECM and LEIM images could distinguish clearly between the platinum foil and epoxy resin although the lateral resolution of LEIM was several ten times as much as that of SECM.
2. SDC, in which a droplet of electrolyte solution can be scanned over the specimen electrode surface, was combined with SECM. T … More he voltammetry and impedance spectra of a polycrystalline gold electrode measured with SDC have revealed that all grains have a (111) orientation but different azimuth angles. SDC was also applied to form locally anodic oxide films on titanium electrode surface. The local formation of anodic oxide film could be evaluated by SECM.
3. A micro silver electrode covered with silver chloride was employed as a probe electrode of SECM. A small mount of chloride ions could be generated locally with a cathodic polarization of the microelectrode, which was named "liquid-phase ion gun". The use of liquid-phase ion gun succeeded in inducing the local breakdown of passive film on iron electrode. The critical amount of chloride ions needed for initiating the local breakdown depended on the film formation conditions, the electric field in film, and pH of solution.
4. The probe current image of titanium electrode in sulfuric acid solution was measured by detecting oxygen which evolved from the electrode in parallel with film formation during anodic polarization. This probe current image coincided with the probe current image obtained with the conventional SECM measurement in which the redox system of ferrocyanide ions was employed as a mediator. Comparison between the probe current images and optical micrograph has indicated that the heterogeneity of oxygen evolution depends on the crystallographic orientation of the substrate titanium and the oxygen evolution takes place preferentially on the thinner passive film or the film with the higher donor density. Less

Report

(3 results)
  • 1999 Annual Research Report   Final Research Report Summary
  • 1998 Annual Research Report
  • Research Products

    (45 results)

All Other

All Publications (45 results)

  • [Publications] K.Fushimi: "Evaluation of Heterogeneity in Thickness of Passive Films on Pure Iron by Scanning Electrochemical Microscopy"ISIJ International. 39. 346-351 (1999)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] A.W.Hassel: "Localized Investigation of Coarse Grain Gold with the Scanning Droplet Cell and by the Laue Method"Electrochim.Acta. 44. 3769-3777 (1999)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] A.W.Hassel: "An Agar-Based Silver/Silver Chloride Reference Electrode for Use in Microelectrochemistry"Electrochemistry Communications. 1. 180-183 (1999)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K.Fushimi: "Heterogeneous Growth of Anodic Oxide Film on a Polycrystalline Titanium Electrode Observed with a Scanning Electrochemical Microscope"J.Electrochem.Soc.. (印刷中). (2000)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K.Fushimi: "Use of a Liquid-Phase Ion Gun for Local Breakdown of the Passive Film on Iron"J.Electrochem.Soc.. (印刷中). (2000)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] 瀬尾眞浩: "走査電気化学顕微鏡による鉄およびチタン表面不働態皮膜の不均一性評価"第122回腐食防食シンポジウム資料,腐食防食協会. 59-66 (1999)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K.Fushimi: "Use of Ion Gun in Liquid Phase for Local Breakdown of Passive Film on Iron"Proceedings of Critical Factors in Localized Corrosion III. PV98-17. 626-634 (1999)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K.Fushimi: "Heterogeneous Growth of Passive Film on Polycrystalline Titanium Electrode-A Scanning Electrochemical Microscope Study-"Proc.8th International Symposium on Passivity. (印刷中). (2000)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] A.W.Hassel: "Localized Investigation and Modification of Passive Materials with the Scanning Droplet Cell"Proc.8th International Symposium on Passivity. (印刷中). (2000)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K.Fushimi: "Study on a Local Breakdown Process of Passive Film on Iron by a Liquid-Phase Ion-Gun"Proc.1999 Joint Meeting of ECS and ECSJ. (印刷中). (2000)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] A.W.Hassel: "Localized Photolectrochemical Measurement with the Scanning Droplet Cell"Proc.1999 Joint Meeting of ECS and ECSJ. (印刷中). (2000)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] A.W.Hassel: "Local Analysis of Anodic Oxide Films on Titanium by Scanning Droplet Cell and Scanning Electrochemical Microscope"Proc.1999 Joint Meeting of ECS and ECSJ. (印刷中). (2000)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] 大川剛史: "多結晶チタン電極表面不働態皮膜の不均一成長"材料と環境'99講演集. 57-60 (1999)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] 伏見公志: "液中イオン銃の開発と鉄不働態皮膜の局部破壊への適用"材料と環境'99講演集. 299-302 (1999)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] 伏見公志: "液中イオン銃による塩化物イオンの局部発生と鉄不働態皮膜の局部破壊"第46回材料と環境討論会講演集. 229-232 (1999)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K. Fushimi, K. Azumi and M. Seo: "Evaluation of Heterogeneity in Thickness of Passive Film on Pure lron by Scanning Electrochemical Microscopy"ISIJ International. 39-4. 346-351 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] A. W. Hassel, M. Seo: "Localized Investigation of Coarse Grain Gold with the Scanning Droplet Cell and by the Laue Method"Electrochim. Acta. 41-21-22. 3769-3777 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] A. W. Hassel, K. Fushimi, M. Seo: "An Agar-Based Silver/Silver Chloride Reference Electrode for Use in Micro-electrochemistry"Electrochemistry Communications. 1-5. 180-183 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K. Fushimi, T. Okawa, K. Azumi, M. Seo: "Heterogeneous Growth of Anodic Oxide Film on a Polycrystalline Titanium Electrode Observed with a Scanning Electrochemical Microscope"J. Electrochem. Soc.. 147-2(in press). (2000)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K. Fushimi, K. Azumi, M. Seo: "Use of a Liquid-Phase lon-Gun for Local Breakdown of the Passive Film on Iron"J. Electrochem. Soc.. 147-2(in press). (2000)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] M. Seo, K. Fushimi: "Evaluation of Heterogeneity of Passive Films Formed on Surfaces of Iron and Titanium by Scanning Electrochemical Microscopy"Proc. 122 nd Symposium of Corrosion and Protection. 59-66 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K. Fushimi, K. Azumi, M. Seo: "Use of Ion Gun in Liquid Phase for Local Breakdown of Passive Film on Iron"Proc. Critical Factors in Localized Corrosion III. PV 98-17. 626-634 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K. Fushimi, T. Okawa, K. Azumi, M. Seo: "Heterogeneous Growth of Passive Film on Polycrystalline Titanium Electrode -A Scanning Electrochemical Microscope Study-"Proc. 8th Internatioanl Meeting on Passivity. (in press). (2000)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] A. W. Hassel, M. Seo: "Localized Investigation and Modification of Passive Materials with the Scanning Droplet Cell"Proc. 8th Internatioanl Meeting on Passivity. (in press). (2000)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K. Fushimi, M. Seo: "Study on a Local Breakdown Process of Passive Film on Iron by a Liquid-Phase Ion-Gun"Proc. Joint Meeting of ECS & ECSJ. (in press). (2000)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] A. W. Hassel, M Seo: "Localized Photoelectrochemical Measurement with the Scanning Droplet Cell"Proc. Joint Meeting of ECS & ECSJ. (in press). (2000)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] A. W. Hassel, K. Fushimi, T. kawa, M. Seo: "Local Analysis of Anodic Oxide Films on Titanium by Scanning Droplet Cell and Scanning Electrochemical Microscope"Proc, Joint Meeting of ECS & ECSJ. (in press). (2000)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] T. Okawa, K. Fushimi, K. Azumi, M. Seo: "Heterogeneous Growth of Passive Film on a Polycrystalline Titanium Electrode"Proc. 1999 Annual Meeting of Jpn. Soc. Corros. Eng.. 57-60 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K. Fushimi, K. Azumi, M. Seo: "Development of an on gun in Liquid Phase and Its Application to Local Breakdown of Passive Film on Iron"Proc. 1999 Annual Meeting of Jpn. Soc. Corros. Eng.. 299-302 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K. Fushimi, M. Seo: "Local Generation of Chloride Ions by an Ion Gun in Liquid Phase and Local Breakdown of Passive Film on Iron"Proc. 46th Meeting of Jpn. Soc. Corros. Eng.. 229-232 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1999 Final Research Report Summary
  • [Publications] K. Fushimi: "Evaluation of Heterogeneity in Thickness of Passive Films on Pure Iron by Scanning Electrochemical Microscopy"ISIJ International. 39・4. 346-351 (1999)

    • Related Report
      1999 Annual Research Report
  • [Publications] A. W. Hassel: "Localized Investigation of Coarse Grain Gold with the Scannig Droplet Cell and by the Laue Method"Electrochim. Acta. 44・21-22. 3769-3777 (1999)

    • Related Report
      1999 Annual Research Report
  • [Publications] A. W. Hassel: "An Agar-Based Silver/Silver Chloride Reference Electrode for Use in Microelectrochemistry"Electrochemistry Communications. 1・5. 180-183 (1999)

    • Related Report
      1999 Annual Research Report
  • [Publications] K. Fushimi: "Heterogeneous Growth of Anodic Oxide Film on a Polycrystalline Titanium Electrode Observed with a Scanning Electrochemical Microscope"J. Electrochem. Soc.. (印刷中). (2000)

    • Related Report
      1999 Annual Research Report
  • [Publications] K. Fushimi: "Use of a Liquid-Phase Ion Gun for Local Breakdown of the Passive Film on Iron"J. Electrochem. Soc.. (印刷中). (2000)

    • Related Report
      1999 Annual Research Report
  • [Publications] 瀬尾眞浩: "走査電気化学顕微鏡による鉄およびチタン表面不働態皮膜の不均一性評価"第122回腐食防食シンポジウム資料,腐食防食協会. 59-66 (1999)

    • Related Report
      1999 Annual Research Report
  • [Publications] K. Fushimi: "Use of Ion Gun in Liquid Phase for Local Breakdown of Passive Film on Iron"Proceedings of Critical Factors in Localized Corrosion III. PV98-17. 626-634 (1999)

    • Related Report
      1999 Annual Research Report
  • [Publications] K. Fushimi: "Heterogeneous Growth of Passive Film on polycrystalline Titanium Electrode - A Scanning Electrochemical Microscope Study -"Proc.8th International Symposium on Passivity. (印刷中). (2000)

    • Related Report
      1999 Annual Research Report
  • [Publications] A. W. Hassel: "Localized Investigation and Modification of Passive Materials with the Scanning Droplet Cell"Proc.8th International Symposium on Passivity. (印刷中). (2000)

    • Related Report
      1999 Annual Research Report
  • [Publications] K. Fushimi: "Study on a Local Breakdown Process of Passive Film on Iron by a Liquid-Phase Ion-Gun"Proc.1999 Joint Meeting of ECS and ECSJ. (印刷中). (2000)

    • Related Report
      1999 Annual Research Report
  • [Publications] A. W. Hassel: "Localized Photoelectrochemical Measurement with the Scannig Droplet Cell"Proc.1999 Joint Meeting of ECS and ECSJ. (印刷中). (2000)

    • Related Report
      1999 Annual Research Report
  • [Publications] A. W. Hassel: "Local Analysis of Anodic Oxide Films on Titanium by Scanning Droplet Cell and Scanning Electrochemical Microscope"Proc.1999 Joint Meeting of ECS and ECSJ. (印刷中). (2000)

    • Related Report
      1999 Annual Research Report
  • [Publications] 大川剛史: "多結晶チタン電極表面不働態皮膜の不均一成長"材料と環境'99講演集. 57-60 (1999)

    • Related Report
      1999 Annual Research Report
  • [Publications] 伏見公志: "液中イオン銃の開発と鉄不働態皮膜の局部破壊への適用"材料と環境'99講演集. 299-302 (1999)

    • Related Report
      1999 Annual Research Report
  • [Publications] 伏見公志: "液中イオン銃による塩化物イオンの局部発生と鉄不働態皮膜の局部破壊"第46回材料と環境討論会講演集. 229-232 (1999)

    • Related Report
      1999 Annual Research Report

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Published: 1998-04-01   Modified: 2016-04-21  

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