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4
Analytical Electron Microscopy
Gianluigi Botton
1 Introduction
The term analytical electron microscopy (AEM) refers to the collection
of spectroscopic data in the transmission electron microscope (TEM)
based on various signals generated following the inelastic interaction
of the incident electron beam with the sample. These signals can be
used to identify and quantify the concentration of the elements present
in the analyzed area, map their distribution in the sample with high
spatial resolution (down to 1 nm or better), and even determine their
chemical state. Although there are several signals generated by the
interaction of primary incident electrons on a sample (Figure 4–1), the
two main techniques at the core of AEM are based on the detection of
X-ray signals generated in the sample by the primary incident electrons
with the technique called energy dispersive X-ray spectroscopy (EDXS)
and the measurement of the energy lost by the incident electrons with
electron energy loss spectroscopy (EELS). These techniques are used
within a TEM (Figure 4–2) equipped with EDXS, EELS detectors, and
other detectors to record TEM images, diffraction patterns, and other
signals that can be combined to form other images containing addi-
tional information on the chemical nature and structure of the sample.
Other techniques such as cathodoluminescence, Auger spectroscopy,
and electron beam-induced current imaging are also part of the arsenal
of techniques available in the TEM but are less frequently implemented
in commercial TEMs or have been used only as proof of concept. Con-
vergent beam electron diffraction has traditionally been considered
one of the AEM techniques, but given the breadth of this topic, the
chapter will focus on the principles of EDXS and EELS, instrumenta-
tion requirements, the quantitative aspects of microanalysis, and the
respective advantages and limitations. Throughout this chapter, several
examples of application of these techniques in practical problems will
be given. A comparison of these AEM methods with other analytical
techniques is presented in a summary. Since this topic has been exten-
sively covered in key detailed early textbook references (Joy et al., 1986;
Williams and Carter, 1996) an update on the current status of the tech-
274 G. Botton
niques will be given based on recent published literature and examples
of work.
1.1 Overview of EDXS
As incident electrons generated by the electron gun in the TEM interact
with atoms and their electrons in the solid, various inelastic processes
are generated. When the primary electron excites bound electrons on
a given shell (Figure 4–3), a core hole is created. This excited state is
created only temporarily and the empty state is therefore fi lled by
electrons from higher energy levels through a deexcitation process by
generation of photons (of suffi cient energy to be considered in the X-ray
Figure 4–1. Signals generated when high-energy incident electrons interact
with a thin sample.
Figure 4–2. Example of
a commercially available
analytical TEM. Visible are
the energy dispersive X-ray
detector, the energy loss
spectrometer, and digital
cameras and detectors.