Chemical State Information of Bulk Specimens Obtained by SEM-Based Soft-X-Ray Emission Spectrometry

Abstract

Electron-beam-induced soft-X-ray emission spectroscopy (SXES) that uses a grating spectrometer has been introduced to a conventional scanning electron microscope (SEM) for characterizing desired specimen areas of bulk materials. The spectrometer was designed as a grazing incidence flat-field optics by using aberration corrected (varied line spacing) gratings and a multichannel plate detector combined with a charge-coupled device camera, which has already been applied to a transmission electron microscope. The best resolution was confirmed as 0.13 eV at Mg L-emission (50 eV), which is comparable with that of recent dedicated electron energy-loss spectroscopy instruments. This SXES-SEM instrument presents density of states of simple metals of bulk Mg and Li. Apparent band-structure effects have been observed in Si L-emission of Si wafer, P L-emission of GaP wafer, and Al L-emissions of intermetallic compounds of AlCo, AlPd, Al2Pt, and Al2Au.

Structural Study of Electrochemically Lithiated Si(111) by using Soft X‐ray Emission Spectroscopy Combined with Scanning Electron Microscopy and through X‐ray Diffraction Measurements

“…The peak position, peak shape, and band centere nergy (53.7 eV) are in good agreement with those in the literature. [20] The Si-L 2,3 spectrum of the fourth layer was exactly the same as that of c-Si, and no peak was observed in the Li-K region, indicatingt hat this layer is the Si(111)s ubstrate.…”

“…The band centere nergy was estimated to be 90.7 eV, which is in good agreement with the literature value. [20] For the Li metal, as ingle peak was observeda t5 4.2 eV in the Li-K region (Figure4c). The peak position, peak shape, and band centere nergy (53.7 eV) are in good agreement with those in the literature.…”

“…The Twop eaks at 89.6 and 92.0 eV as wella so ne broad shoulder around9 6eVw ere observedi nt he spectrum of c-Si (Figure 4b). As the sp 3 hybrid orbital, which is relatedt ot he SiÀSi bond, [19,20] exists in c-Si, the peak observed at 89.6 eV is associated with the low-lying Si 3sÀ3s bonding state, whereas the peak observed at 92.0 eV and the shoulder around9 6eVa re associated with the ss ymmetry components of the sp 3 hybrid orbital. The band centere nergy was estimated to be 90.7 eV, which is in good agreement with the literature value.…”

“…Soft X-ray emissions pectroscopy (SXES) is ap owerful tool to investigate the electronic state of the valence band (VB). [19,20] By using SXES combined with scanning electron microscopy (SEM), we can site-selectivelyo btain information about the electronic state of VB. As compared to the resultsofp reviousreports, [1,2,8] in which the density of state (DOS) for various Li x Si alloys were calculated, the composition of not only c-Li x Si, but also a-Li x Si, can be estimated.…”

Comparison of xenon and gallium sources on the detection and mapping of lithium in Li‐containing materials by using ToF‐SIMS combined FIB‐SEM

“…In SEM-based techniques, wavelength dispersive spectroscopy (WDS) is not suitable whereas only recently very special energy dispersive spectroscopy (EDS) (Hovington et al, 2016) and soft X-ray emission spectroscopy (SXES) detectors are able to detect Li (Terauchi et al, 2014). Electron back scattered diffraction (EBSD) is capable of showing Licontaining phases.…”