Elemental quantification using electron energy-loss spectroscopy with a low voltage scanning transmission electron microscope (STEM-EELS)

Abstract

Electron beam damage in electron microscopes is becoming more and more problematic in material research with the increasing demand of characterization of new beam sensitive material such as Li based compounds used in lithium-ion batteries. To avoid radiolysis damage, it has become common practice to use Cryo-EM, however, knock-on damage can still occur in conventional TEM/STEM with a high-accelerating voltage (200–300 keV). In this work, electron energy loss spectroscopy with an accelerating voltage of 30,20 and 10 keV was explored with h-BN, TiB₂ and TiN compounds. All Ti L_2,3, N K and B K edges were successfully observed with an accelerating voltage as low as 10 keV. An accurate elemental quantification for all three samples was obtained using a multi-linear least square (MLLS) procedure which gives at most a 5 % of standard deviation which is well within the error of the computation of the inelastic partial-cross section used for the quantification. These results show the great potential of using low-voltage EELS which is another step towards a knock-on damage free analysis.