Scanning Electron Microscopy and X-Ray Microanalysis

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Measuring the Crystal Structure


An electron beam incident on a crystal can undergo
electron channeling in a shallow near-surface layer
which increases the initial beam penetration for
certain orientations of the beam relative to the
crystal planes. The additional penetration results in
a slight reduction in the electron backscattering
coefficient, which creates weak crystallographic
contrast (a few percent) in SEM images by which
differences in  local crystallographic orientation
can be directly observed: grain boundaries, defor-
mations bands, and so on (e.g.,. Fig.  8 ).
The backscattered electrons exiting the speci-
men are subject to crystallographic diffraction
effects, producing small modulations in the intensi-
ties scattered to different angles that are superim-
posed on the overall angular distribution that an
amorphous target would produce. The resulting
“electron backscatter diffraction (EBSD)” pattern
provides extensive information on the local orienta-
tion, as shown in. Fig. 8b for a crystal of hematite.
EBSD pattern angular separations provide mea-
surements of the crystal plane spacing, while the
overall EBSD pattern reveals symmetry elements.
This crystallographic information combined with
elemental analysis information obtained simultane-
ously from the same specimen region can be used to
identify the crystal structure of an unknown.


Dual-Beam Platforms: Combined


Electron and Ion Beams


A “dual-beam” instrument combines a fully func-
tional SEM with a focused ion beam (FIB), typi-
cally gallium or argon. This combination provides
a flexible platform for in situ specimen modifica-
tion through precision ion beam milling and/or
ion beam mediated material deposition with
sequential or simultaneous electron beam tech-
nique characterization of the newly revealed
specimen surfaces. Precision material removal
enables detailed study of the third dimension of a
specimen with nanoscale resolution along the
depth axis. An example of ion beam milling of a
directionally solidified Al-Cu is shown in. Fig.  9 ,
as imaged with the SEM column on the dual-
beam instrument. Additionally, ion-beam
induced secondary electron emission provides
scanning ion microscopy (SIM) imaging to com-
plement SEM imaging. For imaging certain speci-
men properties, such as crystallographic
structure, SIM produces stronger contrast than
SEM.  There is also an important class of stand-
alone SIM instruments, such as the helium ion
microscope (HIM), that are optimized for high
resolution/high depth-of-field imaging perfor-
mance (e.g., the same area as viewed by HIM is
also shown in. Fig.  9 ).

a b

BSE MAG: 400 x HV: 20.0 kV WD: 11.0 mm

40 mm

. Fig. 8 a Electron channeling contrast revealing grain boundaries in Ti-alloy (nominal composition: Ti-15Mo-3Nb-3Al-
0.2Si); E 0 = 20 keV. b Electron backscatter diffraction (EBSD) pattern from hematite at E 0 = 40 keV


Scanning Electron Microscopy and Associated Techniques: Overview

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