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.
Laminar and blazed type holographic varied-line-spacing spherical gratings for use in a versatile soft x-ray flat-field spectrograph attached to an electron microscope are designed, fabricated, and evaluated. The absolute diffraction efficiencies of laminar (or blazed) master and replica gratings at 86.00° incidence evaluated by synchrotron radiation show over 5% (or 8%) in the 50-200 eV range with the maxima of 22% (or 26%-27%). Also the resolving power evaluated by a laser produced plasma source is in excess of 700 at the energy near the K emission spectrum of lithium (~55 eV) for all gratings. Moreover, the K emission spectrum of metallic Li with high spectral resolution is successfully observed with the spectrograph attached to a transmission electron microscope.
A new multilayer-coated varied line-spaced grating, JS4000, was fabricated and tested for extending the upper limit of a grating X-ray spectrometer for electron microscopy. This grating was designed for 2-3.8 keV at a grazing incidence angle of 1.35°. It was revealed that this new multilayer structure enables us to take soft-X-ray emission spectra continuously from 1.5 to 4.3 keV at the same optical setting. The full-width at half maximum of Te-L(α1,2) (3.8 keV) emission peak was 27 eV. This spectrometer was applied to indium tin oxide particles and clearly resolved Sn-L(α) (3444 eV) and In-L(β1) (3487 eV) peaks, which could not be resolved by a widely used energy-dispersive X-ray spectrometer.
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