Combining FIB milling and conventional Argon ion milling techniques to prepare high-quality site-specific TEM samples for quantitative EELS analysis of oxygen in molten iron

N. Miyajima, C. Holzapfel, Y. Asahara, L. Dubrovinsky, D. J. Frost, D. C. Rubie, M. Drechsler, K. Niwa, M. Ichihara, T. Yagi

Research output: Contribution to journalArticle

7 Citations (Scopus)

Abstract

Summary This paper reports a procedure to combine the focused ion beam micro-sampling method with conventional Ar-milling to prepare high-quality site-specific transmission electron microscopy cross-section samples. The advantage is to enable chemical and structural evaluations of oxygen dissolved in a molten iron sample to be made after quenching and recovery from high-pressure experiments in a laser-heated diamond anvil cell. The evaluations were performed by using electron energy-loss spectroscopy and high-resolution transmission electron microscopy. The high signal to noise ratios of electron energy-loss spectroscopy core-loss spectra from the transmission electron microscopy thin foil, re-thinned down to 40 nm in thickness by conventional Argon ion milling, provided us with oxygen quantitative analyses of the quenched molten iron phase. In addition, we could obtain lattice-fringe images using high-resolution transmission electron microscopy. The electron energy-loss spectroscopy analysis of oxygen in Fe0.94O has been carried out with a relative accuracy of 2%, using an analytical procedure proposed for foils thinner than 80 nm. Oxygen K-edge energy-loss near-edge structure also allows us to identify the specific phase that results from quenching and its electronic structure by the technique of fingerprinting of the spectrum with reference spectra in the Fe-O system.

Original languageEnglish
Pages (from-to)200-209
Number of pages10
JournalJournal of Microscopy
Volume238
Issue number3
DOIs
Publication statusPublished - 2010 Jun 1

Keywords

  • Argon ion milling
  • Electron energy-loss spectroscopy
  • Focused ion beam milling
  • High pressure and high temperature
  • Laser heated diamond anvil cell
  • Molten iron
  • Oxygen K-edge ELNES
  • TEM
  • TEM sample preparation

ASJC Scopus subject areas

  • Pathology and Forensic Medicine
  • Histology

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  • Cite this

    Miyajima, N., Holzapfel, C., Asahara, Y., Dubrovinsky, L., Frost, D. J., Rubie, D. C., Drechsler, M., Niwa, K., Ichihara, M., & Yagi, T. (2010). Combining FIB milling and conventional Argon ion milling techniques to prepare high-quality site-specific TEM samples for quantitative EELS analysis of oxygen in molten iron. Journal of Microscopy, 238(3), 200-209. https://doi.org/10.1111/j.1365-2818.2009.03341.x