Dose-limited spectroscopic imaging of soft materials by low-loss EELS in the scanning transmission electron microscope

摘要

Spectroscopic imaging in the scanning transmission electron microscope (STEM) using spatially resolved electron energy-loss spectroscopy (EELS) provides one of the few ways to quantitatively measure the real-space nanoscale morphology of soft materials such as polymers and biological tissue. This paper describes the basic principles of this technique and outlines some of the important attributes that define the achievable spatial resolution. Many soft materials can be differentiated from each other as well as from solvents based on their EELS fingerprints. Applying a multiple least squares (MLS) fitting algorithm using such spectral fingerprints to analyze spatially resolved spectrum datasets enables the quantitative mapping of the different components in a specimen. However, in contrast to TEM studies of many inorganic materials where the spatial resolution is limited principally by the spherical aberration of the objective lens, the spatial resolution associated with the imaging of radiation-sensitive soft materials is limited by the total electron dose to which they can be exposed before suffering irrevocable chemical or structural damage. The Rose criterion provides a simple guide to enhance the so-called dose-limited spatial resolution relevant to soft-materials imaging. By using the low-loss portion of an EELS spectrum where the inelastic scattering cross-sections are highest together with improvements in data-collection efficiency and post-acquisition data processing, the dose-limited resolution in spectrum images of solvated polymers has moved into the sub 10 nm regime. This resolution is sufficient to solve important applications-oriented problems associated with hetero interfaces, nanoscale mixing, and nanophase separation.