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Quantitative microanalysis in the analytical electron microscope and its application to the construction of alloy phase diagrams.

Research Project

Project/Area Number 62460195
Research Category

Grant-in-Aid for General Scientific Research (B)

Allocation TypeSingle-year Grants
Research Field 金属材料(含表面処理・腐食防食)
Research InstitutionKyushu University

Principal Investigator

NEMOTO Minoru  Faculty of Engineering, Kyushu University, Professor, 工学部, 教授 (90005265)

Co-Investigator(Kenkyū-buntansha) HORITA Zenji  Faculty of Engineering, Kyushu University, Research Associate, 工学部, 助手 (20173643)
SANO Takeshi  Faculty of Engineering, Kyushu University, Research Associate, 工学部, 助手 (70037810)
MIURA Yasuhiro  Faculty of Engineering, Kyushu University, Associate Professor, 工学部, 助教授 (80037879)
Project Period (FY) 1987 – 1988
Project Status Completed (Fiscal Year 1988)
Budget Amount *help
¥8,300,000 (Direct Cost: ¥8,300,000)
Fiscal Year 1988: ¥400,000 (Direct Cost: ¥400,000)
Fiscal Year 1987: ¥7,900,000 (Direct Cost: ¥7,900,000)
KeywordsAnalytical electron microscope / Quantitative microanalysis / Extrapolation method / Differential X-ray absorption method / k-factor / Ion-milling / Ni-Al-Ta合金状態図 / Ni-Al-Mo三元合金 / Ni-Al-Ta三元合金 / Al-X二元合金 / イオンミリング / 特性X線強度比 / 吸収補正 / 膜厚測定 / ニッケル合金状態図 / 超耐熱合金 / 合金元素の分配
Research Abstract

This study is concerned with the quantitative microanalysis of thin samples in the analyti-cal electron microscope equipped with an energy dispersive spectrometer and its application to the construction of phase diagrams in Ni-based alloys.
For accurate and precise quantification, it is important to use the k-factors which are determined experimentally rather than calculated theoretically. This is because the theoretical equation cannot describe changes in the sensitivity for X-ray detection. The X-ray absorption in the sample leads to a significant error in quntification but this can be corrected simply by using the extrapolation method and the diferential X-ray absorption method, both of which do not require measurement of the thickness in analysed regions.
An experiment shows that the depth distribution of X-ray production is almost constant across the thickness of Ni thin sample. Thus, this effect is considered to be negligible on the quantification Ni-base alloys.
Because the formation of surface layers which are rich in X-element in Al-X (X=Si,Cu,Ag) alloys, an error may be introduced in the quantification particularly for thinner regions. The effects of such surface layer can be reduced by ion-milling or by the use of the extrapolation method.
Determination of the Ni-Al-Ta ternary phase diagrams at lower temperaures results that the gamma/gamma' two phase area expands to the region of higher Ni concentration. This is different from earlier results obtained by EPMA method in SEM. It is found that, in the gamma/gamma' two phase regions of the Ni-Al-Mo ternary system, Mo is more partitioned into gamma' phase than gamma phase when the total amount of Mo is small. However, with an increasing addition of Mo, partitioning behavior is reversed. Mo is more contained in gamma phase than gamma' phase. Similar behavior is observed for Ta in the Ni-Al-Ta ternary system.

Report

(3 results)
  • 1988 Annual Research Report   Final Research Report Summary
  • 1987 Annual Research Report
  • Research Products

    (19 results)

All Other

All Publications (19 results)

  • [Publications] 堀田善治: 日本電子顕微鏡学会分科会,第3回分析電子顕微鏡討論会. 1-6 (1987)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1988 Final Research Report Summary
  • [Publications] 堀田善治: 日本電子顕微鏡学会分科会,第4回分析電子顕微鏡討論会. 1-8 (1988)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1988 Final Research Report Summary
  • [Publications] 堀田善治: 日本電子顕微鏡学会分科会,電子顕微鏡の基礎に関する討論会. 1-6 (1988)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1988 Final Research Report Summary
  • [Publications] Zenji,Horita: Ultramicroscopy. 21. 271-276 (1987)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1988 Final Research Report Summary
  • [Publications] Zenji,Horita: 9th European Congress on Electron Microscopy. 155-156 (1988)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1988 Final Research Report Summary
  • [Publications] Zenji,Horita: Philosophical Magazine. (1989)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1988 Final Research Report Summary
  • [Publications] Zenji,Horita: ISIJ International. (1989)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1988 Final Research Report Summary
  • [Publications] Zenji, Horita: "Simplification of X-ray absorption correction in the thin-sample quantitative microanalysis." Ultramicroscopy. 21. 271-276 (1987)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1988 Final Research Report Summary
  • [Publications] Zenji, Horita: "Determination of local thickness and composition in the analytical electron microscope." 9th European Congress on Electron Microscopy. 155-156 (1988)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1988 Final Research Report Summary
  • [Publications] Zenji, Horita: "Applicability of the differential X-ray absorption method for the determinations of foil thickness and local composition in the analytical electron microscope." Philosophical Magazine. (1989)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1988 Final Research Report Summary
  • [Publications] Zenji, Horita: "Energy dispersive X-ray microanalysis in the analytical electron microscope." ISIJ International. (1989)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1988 Final Research Report Summary
  • [Publications] 堀田善治: 日本電子顕微鏡学会分科会、第4回分析電子顕鏡討論会. 1-8 (1988)

    • Related Report
      1988 Annual Research Report
  • [Publications] 堀田善治: 日本電子顕微鏡学会分科会、電子顕微鏡の基礎に関する討論会. 1-6 (1988)

    • Related Report
      1988 Annual Research Report
  • [Publications] Zenji Horita: Ultramicroscopy. 21. 271-276 (1987)

    • Related Report
      1988 Annual Research Report
  • [Publications] Zenji Horita: 9th European on Electron Microscopy. 155-156 (1988)

    • Related Report
      1988 Annual Research Report
  • [Publications] Zenji Horita: Phillosophical Magazine. (1989)

    • Related Report
      1988 Annual Research Report
  • [Publications] Zenji Horita: ISIJ International. (1989)

    • Related Report
      1988 Annual Research Report
  • [Publications] 掘田善治: Philosophical Magazine.

    • Related Report
      1987 Annual Research Report
  • [Publications] 掘田善治: Proc.9th European Congress on Electron Microscopy.

    • Related Report
      1987 Annual Research Report

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Published: 1987-04-01   Modified: 2016-04-21  

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