Microanalysis using x-ray emission spectrometry (XES) or electron energy-loss spectrometry (EELS) at intermediate voltages should offer advantages over 100kV instruments. Brightness increases linearly with kV (for thermionic sources), but the inelastic scattering cross section decreases. Potential improvements in detectability limit and spatial resolution in both XES and EELS have been major factors spurring the development of intermediate voltage AEMs.The x-ray peak to background ratio increases with kV (Figure 1), and improvements in detectability limits have been reported at 300kV. The variation of detectability with spatial resolution is discussed elsewhere in these proceedings. Beam spreading should decrease linearly with kV, but experimentally the spatial resolution (Figure 2a,2b) does not show the expected improvement. This may be due to increased beam broadening from fast secondary electrons. The smallest probe size consistent with generating sufficient signal (i.e. an FEG) is better than increased kV for improved spatial resolution3. Increased kV has seen the return of the ‘hole count’ problem in XES. Higher voltage electrons generate harder x-rays at the C aperture, and current aperture design cannot sufficiently restrict the xray flux. The flux at 300kV can contribute up to 10% of the characteristic x-ray signal, which severely compromises the microanalysis quality. An FEG with reduced source size may help. At intermediate voltages, intrinsic Ge (IG) detectors can be used for analysis of Kα, lines from high atomic number elements. K line analysis gives improved accuracy compared with L and M line analysis for which Cliff- Lorimer k factors, (both experimental and theoretical) are extremely variable, possibly due to fast secondaries also. IG detectors can detect Au K lines, resolve Kα1Kα2 lines, (see Figure 3) offer improved energy resolution (~120eV) over Si(Li) detectors, and may be more stable under electron irradiation. Continued improvement in IG detectors may result in their displacing Si(Li) detectors from most AEMs.
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