4.0 Article

Development of wavelength-dispersive soft X-ray emission spectrometers for transmission electron microscopes-an introduction of valence electron spectroscopy for transmission electron microscopy

Journal

JOURNAL OF ELECTRON MICROSCOPY
Volume 59, Issue 4, Pages 251-261

Publisher

OXFORD UNIV PRESS
DOI: 10.1093/jmicro/dfq010

Keywords

wavelength-dispersive spectroscopy; soft X-ray emission spectroscopy; transmission electron microscope; valence band; chemical shift; anisotropic soft X-ray emission

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Funding

  1. Ministry of Education, Culture, Sports, Science and Technology of Japan [19051002]
  2. Grants-in-Aid for Scientific Research [19051002] Funding Source: KAKEN

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Two types of wavelength-dispersive soft X-ray spectrometers, a high-dispersion type and a conventional one, for transmission electron microscopes were constructed. Those spectrometers were used to study the electronic states of valence electrons (bonding electrons). Both spectrometers extended the acceptable energy regions to higher than 2000 eV. The best energy resolution of 0.08 eV was obtained for an Al L-emission spectrum by using the high-dispersion type spectrometer. By using the spectrometer, C K-emission of carbon allotropes, Cu L-emission of Cu1-xZnx alloys and Pt M-emission spectra were presented. The FWHM value of 12 eV was obtained for the Pt M alpha-emission peak. The performance of the conventional one was also presented for ZnS and a section specimen of a multilayer device. W-M and Si-K emissions were clearly resolved. Soft X-ray emission spectroscopy based on transmission electron microscopy (TEM) has an advantage for obtaining spectra from a single crystalline specimen with a defined crystal setting. As an example of anisotropic soft X-ray emission, C K-emission spectra of single crystalline graphite with different crystal settings were presented. From the spectra, density of states of pi- and Sigma-bondings were separately derived. These results demonstrated a method to analyse the electronic states of valence electrons of materials in the nanometre scale based on TEM.

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