Scanning transmission electron microscopy (STEM) in combination with electron energy-loss spectroscopy (EELS) can deliver information about variations of bonding at the nm scale. This is typically performed by analyzing the electron-loss near edge structure (ELNES) of given EELS edges. The present paper demonstrates an alternative way of a bonding examination through monitoring the EELS onset positions. Two conditions are essential for their accurate measurement. One (hardware) is using the dual EELS instrumentation that provides near simultaneous acquisition of low-loss and core-loss spectra. Another (software) is the least-square fitting of observed spectra to a reference spectrum. The combination of these hardware and software techniques reveals the positions of EELS onsets with the precision sufficient for mapping tiny variations of bonding. The paper shows that the method is capable of helping to solve practical tasks of nanoscale engineering like the analysis of modern CMOS devices.

Compositional imaging with electron energy loss spectroscopy (EELS) can be performed in both the energy-filtering transmission electron microscope (EFTEM) and in the scanning transmission electron microscope (STEM). Quantitative elemental distributions are obtained from core-edges produced by inner-shell excitations, although more detailed information about chemical bonding and electronic structure is also available from the fine structure associated with valence electron excitations. The fixed-beam EFTEM can provide data from large numbers of pixels very rapidly and offers an advantage for analysis of extended specimen regions containing relatively high atomic concentrations. Acquisition of entire spectra at each pixel in the field-emission STEM (spectrum-imaging technique) provides improved flexibility and accuracy despite the longer recording times. Spectrum-imaging allows post facto data processing with parameters that can be varied after acquisition is completed. In suitably thin specimens, EELS compositional mapping can provide a sensitivity of a few atoms for certain elements.