Methods on Destructive Testing

Scanning Electron Microscopy (SEM)

The scanning electron microscope (SEM) uses a focused

beam of high-energy electrons to generate a variety of signals at
the surface of solid specimens. The signals that derive
from electron-sample interactions reveal information about the
sample including external morphology (texture), chemical
composition, and crystalline structure and orientation of materials
making up the sample. In most applications, data are collected
over a selected area of the surface of the sample, and a 2-
dimensional image is generated that displays spatial variations in these properties. Areas
ranging from approximately 1 cm to 5 microns in width can be imaged in a scanning mode using
conventional SEM techniques (magnification ranging from 20X to approximately 30,000X,
spatial resolution of 50 to 100 nm). The SEM is also capable of performing analyses of selected
point locations on the sample; this approach is especially useful in qualitatively or semi-
quantitatively determining chemical compositions, crystalline structure, and crystal orientations
[CITATION Sus17 \l 1033 ].

I. Application

The SEM is routinely used to generate high-resolution images of shapes of

objects (SEI) and to show spatial variations in chemical compositions: 1)
acquiring elemental maps or spot chemical analyses using EDS, 2) discrimination of
phases based on mean atomic number (commonly related to relative density)
using BSE, and 3) compositional maps based on differences in trace element "activitors"
(typically transition metal and Rare Earth elements) using CL. The SEM is also widely
used to identify phases based on qualitative chemical analysis and/or crystalline
structure. Precise measurement of very small features and objects down to 50 nm in
size is also accomplished using the SEM. Backescattered electron images (BSE) can be
used for rapid discrimination of phases in multiphase samples. SEMs equipped with
diffracted backscattered electron detectors (EBSD) can be used to examine microfabric
and crystallographic orientation in many materials.

II. Limitations

Samples must be solid and they must fit into the microscope chamber. Maximum
size in horizontal dimensions is usually on the order of 10 cm, vertical dimensions are
generally much more limited and rarely exceed 40 mm. For most instruments samples
must be stable in a vacuum on the order of 10-5 - 10-6 torr. Samples likely to outgas at
low pressures (rocks saturated with hydrocarbons, "wet" samples such as coal, organic
materials or swelling clays, and samples likely to decrepitate at low pressure) are
 unsuitable for examination in conventional SEM's. However, "low vacuum" and
"environmental" SEMs also exist, and many of these types of samples can be
successfully examined in these specialized instruments. EDS detectors on SEM's cannot
detect very light elements (H, He, and Li), and many instruments cannot detect elements
with atomic numbers less than 11 (Na). Most SEMs use a solid state x-ray detector
(EDS), and while these detectors are very fast and easy to utilize, they have relatively
poor energy resolution and sensitivity to elements present in low abundances when
compared to wavelength dispersive x-ray detectors (WDS) on most electron probe
microanalyzers (EPMA). An electrically conductive coating must be applied to electrically
insulating samples for study in conventional SEM's, unless the instrument is capable of
operation in a low vacuum mode.

III. Operation

In an SEM, an electron beam is emitted from an electron gun, then narrowed to a

size of approximately 0.4-5 nm in diameter through the use of one or two condenser
lenses. The beam then passes through a pair of deflection coils in the electron column to
deflect the beam in the x and y axes before interacting with the sample. This deflection
ensures that the scan is in a raster fashion, which means it is a rectangular image
capture pattern of the sample. When the electron beam interacts with the sample, it
loses energy due to random scattering and absorption by the sample. 

Figure 1. Schematic of how an SEM works (Figure courtesy of Creative Commons)

The electron beam of a scanning electron microscope interacts with atoms at
different depths within the sample to produce different signals including secondary
electrons, back-scattered electrons, and characteristic X-rays. Each of these signals has
its own detector in the SEM, as seen in Figure 1. Secondary electrons are low energy
electrons that are ejected from the valence or conduction bands of atoms in the sample
through inelastic scattering from the beam electrons. Back-scattered electrons are
electrons from the beam that are reflected through elastic scattering interactions with
atoms in the sample. The intensity of the back-scattered electron signal is dependent
 upon the atomic number so it can provide information about the distribution of different
elements in a sample. The characteristic X-rays are emitted when the electron beam
interacts with the sample and removes an inner shell electron, resulting in a higher-
energy electron filling the shell and releasing energy. The energy or wavelength of these
X-rays can be measured by Energy-dispersive X-Ray Spectroscopy to identify and
measure the abundance and distribution of elements in the sample. The electron beam
absorbed by the sample is detected and used to create an image of the sample
distribution. The resulting image is a map displaying the intensity of signal emitted from
the area of the sample being scanned, as seen in Figure 2. Additionally, EDS detectors
can be attached to the SEM for elemental analysis.

In order to obtain SEM images, the sample

must be electrically conductive at the surface as well as
electrically grounded so that it does not accumulate
charge. Samples are mounted onto the specimen
holder using a conductive adhesive. Metal samples
require minimal sample preparation other than
conductively mounting the sample to the stage. Non-
conductive materials typically undergo ultrathin coating
with electrically conductive materials such as gold,
platinum, chromium, or graphite. The coating is
accomplished through sputter-coating or evaporation
Figure 2. SEM image of pollen grains. Image
under high vacuum. released to the public domain by original author
Dartmouth College Electron Microscope Facility
Different SEM images can be produced based on the type of detector being used
and these image can be used to see what the sample looks like on the nanoscale. The
most typical detector used detects the secondary electrons that are emitted from the
sample by inelastic scattering. The number of secondary electrons detected represents
the signal intensity and is combined with the position of the beam to produce a gray-
scale images showing the sample's topography, as seen in Figure 2. Back-scattered
electrons can also be used to get an image since elements will reflect a different number
of electrons. Therefore, the intensity of back-scattered electrons will vary throughout a
sample depending on the elements present. An SEM image produced from the intensity
of back-scattered electrons and the beam position can show the distribution of different
elements in the sample. Elements that are heavier and reflect more electrons will appear
brighter in the image so back-scattered electrons can show contrasts in chemical
composition. However, the identity of the different elements cannot be determined with
SEM alone, an EDS attachment would have to be used to quantify the relative
abundance of different elements [ CITATION Emi20 \l 1033 ].

IV. Advantage
V. Disadvantage

VI. Standard

ASTM Standards in the SEM

The goal of image analysis in microscopy is the quantification of the

microstructure. To this end, there are many ASTM standards that specify procedures in
microscopy, and several of them are either specific to electron microscopes or apply to
both electron- and light-optical microscopes. The standards listed below are all under the
jurisdiction of ASTM Committee E04 on Metallography [ CITATION Fri03 \l 1033 ].

E 562 provides the statistical basis for point counting a discrete phase. It supplies
guidance on sample selection and preparation, and it provides tables to determine the
required number of points and fields to achieve a given level of precision. The standard
also includes measures of precision and bias based on interlaboratory round-robin
testing. Although it was written for manual measurement, automatic image analysis (AIA)
can be used, and the measurements can be made directly on a microscope or
photomicrograph.

E 766 is a standard practice for calibrating the magnification of an SEM. During

its last revision in 1998, it was broadened to permit the use of any magnification
calibration standard. The procedure describes calibration in both the x- and y-directions
as well as calibration of the scale marker. A table is provided for recording the data.

E 986 is a standard practice for SEM beam size characterization. It describes an

experiment for measuring the electron beam diameter with suitable precautions to
achieve reproducible results. During its recent revision in 2002, the standard was
updated to incorporate digital microscopes.

E 1245 describes stereological measurements and quantification of the amount

and distribution of inclusions or second phase particles in a matrix. It describes sample
selection, preparation, and system calibration. The method is designed for AIA, and it
reports: NA, NL, AA, average area, average length, and mean free path. The 95%
confidence interval and %relative accuracy are also calculated. This standard is
applicable to many types of microstructures, and it produces results of known precision.

E 1268 is a method for assessing the degree of banding or orientation within a

microstructure. It requires measurements to be made on two perpendicular axes and
reports an anisotropy index (AI) and a measure called Ω12. It also contains
photomicrographs of various microstructures to illustrate the applicability of the method.
E 1508 is a standard guide to quantitative analysis by EDS. Although the guide is
not intended to replace a textbook on microanalysis, it suggests good operating practice.
Parameters that are under control of the analyst are identified, and guidance on their use
 is provided. The standard also reports precision and bias based on an interlaboratory
round-robin testing program, using both standards and standardless methods.

E 2142 is a standard that was published in 2002 after several years of

development. This standard calls for the use of SEM/EDS to analyze inclusions in steel,
but it is applicable to other discrete phases as well. As steelmaking practice produces
steels with fewer inclusions, the LOM is not always adequate to characterize their size
and shape, and certainly not their composition. In this case, the SEM is used for its
higher resolution, and EDS provides the chemical composition. In the most commonly
used inclusion rating standard (E 45), the chemistry of inclusions is inferred from their
shape or reflectivity. Now E 2142 makes a direct determination of composition and
provides for either a traditional classification or a user-defined one. The traditional
classification of inclusions is: types A, B, C, and D, which are inferred to be sulfides,
aluminates, silicates, and globular oxides respectively, but in E 2142, the automated
chemical classification program of the EDS computer is set up to suit the application.
Complex or duplex inclusions analyzed by this method tend to be resolved into their
components, especially at higher magnifications.

TABLE 1. Designation and brief description of some ASTM standards for use in
the SEM
ASTM Designation Applicability Brief description
E 562 LOM/SEM Point counting
E 766 SEM Magnification calibration
E 986 SEM Beam diameter
measurement
E 1245 LOM/SEM Stereological measurement
of discrete phases
E 1268 LOM/SEM Degree of banding
E 1508 SEM Guide to quantitative
analysis by EDS
E 2142 SEM Classifying inclusions by
SEM/EDS

References:

Friel, J. (2003). ASTM Standards in the SEM. Microscopy and Microanalysis, 9(S02), 72-73.

doi:10.1017/S1431927603440282

Nagle, E. (2020, May 7). Scanning electron microscopy (SEM). Retrieved November 18, 2020, from
Chemistry Libre Texts:
https://chem.libretexts.org/Courses/Franklin_and_Marshall_College/Introduction_to_Materials
_Characterization__CHM_412_Collaborative_Text/Electron_and_Probe_Microscopy/Scanning_e
lectron_microscopy_(SEM)
Swapp, S. (2017, May 26). Scanning Electron Microscopy (SEM). Retrieved November 18, 2020, from
Science Education Resource Center:
https://serc.carleton.edu/research_education/geochemsheets/techniques/SEM.html